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Nano-engineering coatings and thin films

“Nano-engineered coatings and thin films symposium” will be the proposed new title of the former 2015 symposium EE on “Protective Coatings and Thin Films” one. Emphasis will be given to the development of new thin films for mechanical, tribological, optical, biological and energy-based applications.


For almost 40 years, hard and wear-resistant thin-films and coatings played vital roles in improving the performance of a variety of tools, machine parts, and innumerous devices. Moreover, the concept and practice of tailoring the structure and morphology of a given coating or thin film system to modify its properties has been long used to add new functionalities and improved behavior to several materials and devices. However, the development of new products and the need to enhance materials functionalities requires the optimization of the coating or thin film system to respond to the increasing demands of a targeted application. Nano-engineering of surfaces is playing a fundamental role in this particular area of research, either in the case of new materials development or in their modification. This symposium will be dedicated to advanced methods of vapor deposition and surface nano-engineering, as well as to nanoscale methods of materials characterization. Areas of particular interest will include, but not limited to, the following topics:

  • Fundamentals of vapor-based deposition processes, growth modeling, plasma-surface interactions and in situ diagnostics;
  • New deposition processes, including HIPIMS technology, liquid-based deposition, thermochemical heat treatments like plasma nitriding + PVD, PACVD deposition, or on the use of hybrid methods combining for instance arc evaporation and magnetron sputtering or PVD and CVD, atmospheric plasma, and related approaches;
  • Nanostructured coatings or nano-engineered thin film architectures, including nanocomposites, multilayers, nanolayers and glancing angle deposition;
  • Correlation between micro- and nanostructure and functional properties such as optical, electrical, mechanical, tribological, thermoelectrical, thermochromic, magnetic, etc.;
  • Hard, wear and corrosion/oxidation resistant coatings;
  • Characterization methods to determine the properties of thin films and coatings in their in-service severe conditions;
  • In-situ characterization;
  • Microstructural multiscale: advanced modes of characterization (EELS, tomography, etc.);
  • Thin films for smart application: (bio)sensors; biocompatibility; energy; etc.;
  • New trends in thin film materials: metallic glasses; high entropy alloys, oxynitrides, intermetallics, plasmonics, etc.;

We call for communications giving the latest information on research and development in topics corresponding to one or more of the above-mentioned areas.

Hot topics to be covered by the symposium:

  1. Fundamentals of thin film growth: diagnostics, analysis and modeling; in situ film growth characterization;
  2. Surface modification/functionalization;
  3. High Power Impulse Magnetron Sputtering processes;
  4. Atmospheric processes - organic synthesis and surface functionalization;
  5. Characterization methods at the nanoscale of nano-engineered thin films;
  6. Corrosion and oxidation resistant coatings;
  7. Low-friction, self-healing, self-lubricant and wear resistant coatings;
  8. Design of novel thin films for energy conversion, saving and storage;
  9. Coatings with surface Plasmon resonance behavior;
  10. Coatings for biological applications;
  11. New energetic plasma processes and related advanced hard coatings.

List of invited speakers:

  • Ivan Petrov (USA) – “Control of micro and nanostrucutre - recent advances"
  • Ulf Helmersson (SWE) – “Vapor phase nanoparticle synthesis
  • J. Patscheider (CHE) – “Oxynitride coatings: New opportunities to profit from and challenges to master” FV
  • Peter Panjan (SVN) – “Tribological aspects related with PVD hard coating morphology
  • J.F. Pierson (FRA) – “Copper oxides: low cost and earth abundant material for energy applications
  • Alberto Palmero (ESP) – “Porous nanostructured coatings grown by PVD techniques: from fundamentals to devices
  • J. Schmitz (NLD) – “Low temperature thin films for next-generation microelectronics” FV
  • Thierry Epicier (FRA) – “Opportunities to characterize thin films by advanced TEM” PhS
  • Gerry van der Kolk (NLD) – “Influence of plasma conditions on nanocomposite and nanolayered coatings”
  • Rostislav Daniel (AUT) - “Fracture Toughness Enhancement of Thin Films by Advanced Microstructural Design and Architecture”
  • Sven Ulrich (DEU) – “State of the art of thin film Lithium ion batteries and their application potential“

Scientific committee:

  • G. Abadias (France)
  • C. Mitterer (Austria)
  • J.C. Sanchez-Lopez (Spain)
  • A. Cavaleiro (Portugal)
  • J-H. Huang (Taiwan)
  • J. Schmitz (Netherlands)
  • A. Anders (USA)
  • T. Nyberg (Sweden)
  • T. Belmonte (France)
  • R. Smith (UK)
  • B. Podgornik (Slovenia)
  • P. Patsalas (Greece)
  • M. A. Djouadi (France)
  • A. Kromka (Czech Republic)
  • D. Depla (Belgium)
  • N. Martin (France)
  • R. Cremer (Germany)
  • S. M. Aouadi (USA)
  • D. Mariotti (UK)
  • K. Sarakinos (Sweden)
  • S. Kassavetis (Greece)
  • J. Borges (Portugal)
  • P.H. Mayrhofer (Austria)
  • M. Cekada (Slovenia)
  • L. Zajickova (Czech Republic)
  • M. Braic (Romania)

The proceedings will be published in the journal "Surface and Coatings Technology" (Elsevier).

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Fundamentals of thin film growth: diagnostics, analysis and modeling 1 : Kostas Sarakinos + Ivan Petrov
Authors : Ivan Petrov, G. Greczynski, J. Rosen, J. Birch, L. Hultman, J.E. Greene
Affiliations : Frederick Seitz Materials Research Laboratory and Materials Science Department, University of Illinois, Urbana, Illinois 61801; Department of Physics (IFM), Linköping University, SE-581 83 Linköping, Sweden

Resume : Polycrystalline TiN and related transition-metal nitride (TMN) thin films are typically deposited by reactive magnetron sputter deposition and employed as diffusion barriers in microelectronics as well as hard, wear-, and corrosion-resistant coatings in mechanical and optical applications. We will review the fundamental film growth processes - nucleation, coalescence, competitive growth, and recrystallization - and their role in thin film microstructure evolution as a function of substrate temperature. Special attention will paid to in-situ substrate treatment by ion-irradiation and its effect on film microstructure and adhesion. We will also review recent advances in the selective use of metal ions during HIPIMS co-sputtering to extend the attainable structures and properties in metastable TMN with examples of Ti(1-x)AlxN, Ti(1-x)SixN, ad Ti(1-x)TaxN. We probe the effects of (i) metal versus rare-gas ion irradiation as well as (ii) the type of metal ion uses (Ti vs Me). We employ a metastable NaCl-structure Ti0.39Al0.61N as a model system to demonstrate that switching from Ar+- to Al+-dominated bombardment eliminates phase separation, minimizes renucleation during growth, reduces the high concentration of residual point defects, and thus results in dense, single-phase, stress-free films. With the TiTaN system we show that synchronized pulsed ion bombardment in the hybrid system with the heavy-metal ions (Ta) permits to grow dense, hard, smooth, and stress-free thin films at lowered substrate temperature, with no external heating.4 Overall, we demonstrate that using synchronous bias to select the metal-rich portion of the ion flux opens new dimension for ion-assisted growth in which momentum can be tuned by selection of the metal ion in the hybrid/cosputtering configuration and stresses can be eliminated/reduced since the metal ion is a component of the film. We begin to apply the same comprehensive approach to Transition Metal Diborides (TMB2) TMB2 have many desirable physical and mechanical properties such as a high melting point, good thermal and electrical conductivity, high hardness, high wear- and corrosion resistance, as well as excellent chemical stability at elevated temperatures. A common problem in sputter-deposited MiBx layers is that the film contains excess boron with x ranging from 2.4 to 3.5. It is important to be able to control the B/TM ratio during film growth as a first step to synthesizing epitaxial single crystal films in order to investigate their fundamental properties. We use TiBx as a model system and study the effect of the discharge pressure and plasma density on the B/Ti ratio during magnetron sputtering of a TiB2 target. We present results from establishing control of the B/Ti ratio in magnetron sputter-deposited TiBx thin film and to synthesize stoichiometric single crystalline TiB2 layers.

Authors : Bo Lü1, Georgios Almyras1, Joseph E. Greene2,3, Kostas Sarakinos1
Affiliations : 1 Nanoscale Engineering Division, Department of Physics, Chemistry and Biology, Linköping University, SE 581 83, Linköping, Sweden 2 Thin Film Physics Division, Department of Physics, Chemistry and Biology, Linköping University, SE-581 83 Linköping, Sweden 3 Materials Science and Physics Department, University of Illinois, Urbana, Illinois, USA

Resume : Condensation of vapor on weakly interacting substrates leads to formation of 3D atomic islands via the process of de-wetting. While it is widely accepted that this process is driven by surface energy minimization, it is currently not understood how 3D island formation and evolution occurs at an atomistic level. Seeking to achieve this understanding, in this work we employ kinetic Monte-Carlo simulations that describe— in a fully atomistic fashion—growth of Ag on weakly interacting FCC-structured substrates. Our data reveal the following chain of atomic events that lead to compact 3D island shapes: 3D nuclei are first formed due to facile step ascent at the substrate level, followed by microfaceting on the sides of the 3D island, which in turn facilitate upward diffusion from the island base to its summit. Furthermore, our results highlight differences in periphery diffusion around strongly faceted and monolayer islands, with indications of a new type of corner-crossing diffusion anisotropy that promotes the growth of (100) facets over (111) for certain temperatures.

Authors : E. Aschauer1, S. Sackl2, C.M. Koller1, T. Schachinger3, M. Arndt4, P. Polcik5, H. Riedl1,6, and P.H. Mayrhofer1,6
Affiliations : 1Christian Doppler Laboratory for Application Oriented Coating Development, TU Wien, Austria 2 Department of Physical Metallurgy and Materials Testing, Montanuniversität Leoben, Austria 3 Technische Universität Wien, University Servicecenter for TEM (USTEM) Vienna, Austria 4Oerlikon Balzers, Oerlikon Surface Solutions AG, Liechtenstein 5Plansee Composite Materials GmbH, Germany 6Institute of Materials Science and Technology, TU Wien, Austria

Resume : To face the challenges of modern manufacturing techniques and advanced technologies, material design in the atomic scale range is imperative. 2D-nano composite coatings deposited by PVD are a highly effective way to increase the limited properties of bulk materials, such as thermal stability, oxidation or wear resistance. PVD arises the possibility to combine coating materials with contrary properties such as hardness and toughness, or thermal stability with self-lubrication to gain revolutionary characteristics. Our newly developed Ti-Al-N/Mo-Si-B multilayer thin films provide the possibilities of outstanding mechanical properties combined with superior oxidation behaviour, especially in the high temperature regime. However, to gain a deeper understanding on the thermo-mechanical properties and the reaction kinetics during thermal exposure, a set of high resolution techniques, including high resolution transmission electron microscopy, electron energy loss and energy-dispersive X-ray spectroscopy, as well as selected area diffraction, compared to atom probe tomography are used for an in-depth analysis. Therefore, a comprehensive analysis of our nano-laminated coatings in the as deposited state and after thermal treatments in vacuum and air up to 1600 °C was carried out. The correlation between the hardness, morphology, chemical composition, as well as structure allocates a distinct knowledge on the diffusion process and phase transformations at elevated temperatures.

Authors : Jean-Thomas Fonné, Emmanuelle Gouillart, Hervé Montigaud, Ekaterina Burov, Sergey Grachev, Damien Vandembroucq
Affiliations : Surface du Verre et Interfaces, Joint Unit CNRS/Saint-Gobain UMR125, Aubervilliers, France;;;; Laboratoire PMMH, UMR 7636 CNRS/ESPCI Paris/Univ. Paris 6 UPMC/Univ. Paris 7 Diderot, 10 rue Vauquelin, 75231 Paris cedex 05, France

Resume : In the glazing industry, silica thin films are used in low-emissivity stacks as a diffusion barrier for alkalis. However, diffusion mechanisms resulting from the high-temperature interaction between thin films and the glass substrate are poorly understood. We study the interdiffusion between PVD-sputtered aluminum-doped silica thin films, and their float-glass substrates, at temperatures close to or slightly above the glass transition of the substrate. In order to characterize concentration profiles of the different species following thermal treatments, we use Secondary Ion Mass Spectroscopy (SIMS) measurements, together with XPS and EMPA. We observe several diffusive mechanisms, with different kinetics. In a first stage, alkalis (sodium and potassium) diffuse rapidly from the glass substrate to the silica layer, and their concentration stabilizes quickly. When varying the aluminum content of the silica layer, we observe that the alkali content increases linearly with the aluminum content. Since the addition of alkalis decreases significantly the glass transition of the Al-doped silica layer, interdiffusion profiles are then observed between the silica layer and the glass substrate. However, we observe that the effective diffusion coefficient varies locally, and decreases when the aluminum concentration increases. The different diffusion lengths observed for the different elements reveal multicomponent diffusion effects, that are characteristic of silicate glasses.

Authors : C. Furgeaud, L. Simonot, A. Michel, C. Mastail, G. Abadias
Affiliations : Institut Pprime, UPR 3346, Université de Poitiers-CNRS-ENSMA, France

Resume : Developments in microelectronics require a continuous improvement of device performance and a downscaling of constitutive features. Currently, these devices integrate metallic layers, often deposited by DC magnetron sputtering, whose microstructure, morphology and intrinsic stress are intimately correlated to the elementary growth mechanisms. Indeed, as the lateral grain size is usually set-in during coalescence stage, controlling the nucleation conditions is a main aim of growth studies. In this work, we combine three in situ and real-time measurements, during metallic thin film growth, namely multiple-beam optical stress sensor (MOSS), electrical resistance and surface differential reflectance spectroscopy (SDRS). This unique coupling allows an in-depth understanding of the early growth stages which strongly influence morphology and crystalline structure, as studied by ex situ AFM, TEM and XRD. Illustrations will be given for high mobility metals, such as Ag, Cu and Au, following a Volmer-Weber growth with a complex compressive-tensile-compressive stress behavior. Our methodology gives access to characteristic lengths like percolation thickness and onset of film continuity. Influence of chemical interactivity was studied using different buffer layers. A detailed study on post-growth relaxation phenomena reveals importance of kinetic effects. Thus, this combination of in situ diagnostics enables a better understanding of pre- and post-coalescence mechanisms during high-mobility metal growth.

Authors : Julio Gutiérrez Moreno, Michael Nolan
Affiliations : Tyndall National Institute, University College Cork, Lee Maltings, Dyke Parade, Cork, Ireland

Resume : TiN is widely used in industry and a promising candidate for sensor devices due to its good conductivity, ultra-hardness, resistance to corrosion, biocompatibility and compatibility with standard microelectronics fabrication methods. Nevertheless, TiN can spontaneously form a thin oxide layer when it is exposed to air or typical biosensing atmosphere, which could enhance adsorption of bio-molecules and deteriorate the properties of TiN. Therefore, there is interest in studying the biofouling of TiN to find strategies to inhibit this process. In this work, we carried out density functional theory (DFT) simulations of the TiO2-TiN interface as a model of the oxide layer on TiN. An interface of rutile (110) and TiN (100) shows small lattice mismatch. The energy costs for the formation of defects like Ti vacancies in the substrate (Evac=4.0 eV) or O vacancies in the oxide (Evac=3.9 eV) are quite high, even in the interface region. The formation of an oxynitride structure in the interface region is more favourable (1.2 eV relative to oxide-on-nitride interface). Our DFT+U (with Hubbard U to localise Ti 3d states in the oxide) study shows the presence of Ti 3+ atoms in the TiO2 region. Finally, we have investigated the adsorption of amino acids (that make up peptides present in proteins) on the oxide in the TiO2-TiN interfacial system. Glycine in its zwitterion form exhibits stronger adsorption onto the rutile TiO2 (110) – TiN (100) interface model surface (Eads=-1.5 eV) compared to bare TiN (E=-0.4 eV), but similar to pure rutile (110), where Eads = -1.7 eV; the -COO group is the most favorable group for adsorption. These results will give us a deeper understanding of oxidised TiN and how this is related with the biofouling process and can be used as a guide to rationally design novel anti-biofouling coating materials.

Authors : C. Mastail, F. Nita, A. Michel, G. Abadias
Affiliations : Institut Pprime

Resume : Due to their combination of covalent, ionic and metallic bonding, transition metal nitride (TMN) thin films find applications in various technological fields, ranging from hard and protective coatings for cutting tool, diffusion layers in microelectronics, contact electrodes in solar cell applications. Depending on the deposition conditions, TMN thin films may be synthesized with different structural properties: bi-phase nanocomposite, metastable cubic solid solution or columnar thin film. As it allows tailoring unique film microstructures, Oblique Angle Deposition (OAD) receives an increasing popularity [1]. OAD is a way to architecture the growing layer and in turn to control film properties, such as texture, porosity, anisotropy. However, predicting the microstructure still remains a challenging problem. In this context, predictive design can be achieved by using multi-scale computational approaches based on kinetic Monte Carlo (kMC) algorithm [2] to mimic real deposition conditions, and gain insights on understanding the competitive columnar growth and texture evolution in TiN-based films. The present work gives some simulation results for reactive magnetron sputtering at OAD. The influence of the most important experimental parameters (substrate temperature, deposition pressure, incident angle and deposited energy of some incoming particles) will be discussed regarding the resulting thin film morphology (porosity, surface roughness, columnar tilt angle, layer density) [1] A. Barranco, et al. Progress in Materials Science 76 (2016) 59-153 [2]. Nita, et al., Physical Review B 93 (2016) 064107

Authors : F. Cemin 1, G. Abadias 2, C. Furgeaud 2, A. Michel 2, T. Maroutian 3, P. Lecoeur 3, T. Minea 1, D. Lundin 1
Affiliations : 1 LPGP, UMR 8578 CNRS, Université Paris-Sud, Orsay, France; 2 Institut Pprime, UPR 3346 CNRS, Université de Poitiers, Poitiers, France; 3 C2N – Orsay, UMR 9001 CNRS, Université Paris-Sud, Orsay, France;

Resume : Copper has attracted much interest as an ultrathin film material for nano-ranged downscaled electrical, electronic, and magnetic devices due to its low electrical resistivity and good electromigration resistance. Continuous efforts are being made in terms of increasing the performance of such devices, which is strongly dependent on the crystalline structure, electrical properties, and growth process of Cu films. High power impulse magnetron sputtering (HiPIMS) has recently showed great promise as an interesting plasma-based deposition technology for growing such ultrathin films. This deposition method allows a much higher ionization fraction of the sputtered vapor leading to better control of the film properties, as compared to conventional direct current magnetron sputtering (DCMS). In this work, we have grown high-quality Cu thin and ultrathin films with high electrical conductivity, low compressive intrinsic stress, large-grained compact microstructure, and different textures by using a HiPIMS deposition process and substrate biasing. We found that the electrical resistivity of the as-deposited ultrathin Cu films was reduced by ~30% when deposited by HiPIMS compared to DCMS, which was associated to an increase in the grain size. We also show a new route to grow epitaxial ultrathin Cu films on Si(001) wafers without any prior chemical or plasma etching. Intrinsic stress evolution during Cu films growth is investigated and correlated to the early stages of film formation.

Authors : James A. Grant-Jacob, Stephen J. Beecher, David P. Shepherd, Robert W. Eason, and Jacob I. Mackenzie
Affiliations : Optoelectronics Research Centre, University of Southampton, Southampton SO17 1BJ, UK

Resume : To date, pulsed laser deposition (PLD) has been used for depositing many different materials under the classes of metals, semiconductors, and dielectrics. For the latter, PLD is advantageous for fabrication of crystalline layers that are suitable for high quality planar waveguides. In previous work, we showed PLD can be exploited for fabricating garnet-crystal layers, specifically Yb:YAG, with optical quality close to Czochralski grown material [1]. Typical growth rates are slow at < 1 microns per hour but some progress has been made increasing depositions using a pulsed laser operating at a repetition rate of 20 Hz [2]. Here, we report a ~ 5 x increase in growth rate from previous work, demonstrating that YGG and YAG can be grown with excellent crystal quality at deposition rates approaching 20-microns per hour by using an excimer laser operating at a repetition rate of 100 Hz. This surprising result demonstrates the unique capability of PLD at 100 Hz, for upscaling deposition speeds to a rate that is industrially relevant for thick films. 1. Stephen J. Beecher et al. Proc. SPIE 9726, Solid State Lasers XXV: Technology and Devices, 97261Z (March 16, 2016) 2. J. A. Grant-Jacob et al. Opt. Mater. Express 6, 91-96 (2016)

Authors : Daniel Pelati (1,2), Andrea Cattoni (1), Stéphane Collin(1), Jean-Christophe Harmand (1), Frank Glas (1), Phannara Aing (2), Fabrice Oehler (1)
Affiliations : (1) C2N, CNRS – Univ. Paris-Sud – Université Paris-Saclay, Site de Marcoussis - 91460 Marcoussis, France ; (2) Riber SA, 95870 Bezon, France

Resume : Many semiconductor-based devices require a mono-crystal. Yet, out of the volume of a wafer only the final micron is useful for the actual device fabrication or epitaxy. The rest plays no other role than mechanical support while it has the same purity and cost. We investigate here the potential of a low temperature technique to obtain thin (~20nm) mono-crystalline patches of germanium on glass, based on of the peculiar properties of Al/Ge bilayers. The presence of Al next to amorphous Ge material substantially lower the Ge crystallization temperature from ~500°C down to ~250°C. This process can be further enhanced by engineering a GeOx/AlOx barrier between the two materials so that the final Ge crystals exhibit a near complete 111 orientation. The dynamics of the 111-oriented crystallization process are not well understood as other phenomena (parasitic growth, segregation) may compete with the main process. By combining (diffraction limited) in-situ optical microscopy with an oven operating at 200-400°C under nitrogen, we are able to measure in real time the initiation and the propagation of the crystallization on 20nm thick Ge layers. We then correlate these kinetics to the micro-structure of the sample measured by ex-situ TEM, XRD and EBSD. The chemistry of the AlOx/GeOx diffusion barrier, air or plasma oxidation is determined to be a crucial parameter. The obtained Ge crystalline patches are good candidates for a subsequent epitaxy of GaAs or Ge by MBE or MOCVD.

Fundamentals of thin film growth: diagnostics, analysis and modeling 2 : F.Vaz + J. Schmitz
Authors : Gerry van der Kolk, Ivailo Dolchinkov
Affiliations : Ionbond Netherlands b.v.

Resume : A broad range of diamond like carbon coatings has found its application in the industry. Initially the majority of the DLC coatings has been hydrogenated DLC (a-C:H). It is common practice to design a multilayer coating with individual layers, with as main function to reduce the overall internal stress in the coating. The mechanical properties can also be influenced by doping hydrogenated DLC coatings with carbide forming elements, 3d, 4d, 5d transition metals and B or Si. It has been demonstrated that especially impact fatigue can be increased if a proper period is taken in the range of a few nm. Non hydrogenated DLC coatings (ta-C) have so far been applied mainly as a single layer. In this paper we show the nano-layering of a homogeneous ta-C coating, whereby the varying parameter is the sp2/sp3 ratio. This variation has been achieved by extreme plasma conditions. We have further seen that allthough the overall hardness is less than that of a homogeneous film, that the mechanical wear properties are superior. Furthermore we will show nanocomposite coatings whereby hydrogenated W-doped a-C:H is compared with non hydrogenated W doped taC. HR-TEM pictures show that the growth mechanism is different for hydrogenated versus non-hydrogenated doped DLC.

Authors : Han-Yin Liu, Ching-Sung Lee, Wei-Chou Hsu, Guan-Jyun Liu, Ruei-Chin Huang, Wei-Hsin Liu, Fu-Yuan Hou, and Guan-Cheng Tu
Affiliations : Department of Electronic Engineering, Feng Chia University, Taichung City, Taiwan

Resume : This work proposes a solution-based chemical vapor deposition technique known as mist chemical vapor deposition (Mist-CVD) to grow TiO2 thin films. The isopropyl titanate was dissolved in the methanol as a precursor solution. The precursor solution was misted by an ultrasonic vibration generator. The misted precursor solution was transported to a substrate by N2 flow. The TiO2 film was deposited on the substrate which is heated to 350oC. Different crystal phases of the TiO2 thin films were synthesized by post deposition annealing technique with different annealing temperature. It was found that the annealing temperature affects the crystal phase of the TiO2. The anatase, rutile, and mixed phases of the TiO2 films were synthesized by post deposition annealing (PDA) process at 400oC, 800oC, and 650oC, respectively. The TiO2 film was characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectrum and photoluminescence (PL). The XPS provides quantitative and qualitative analyses of the TiO2 films. The binding energy of Ti is different among the anatase-, rutile-, and mixed-phase TiO2 films. The results of XRD indicate that the TiO2 films with PDA process at 400oC, 650oC, and 800oC are anatase, mixed, and rutile phase, respectively. The Raman shift is used to observe the structures of the TiO2 films. The material defects of the TiO2 films are characterized by the PL spectrum. It was found that the TiO2 with 800oC PDA process has insignificant intensity in PL spectrum. This result suggests that higher annealing temperature is helpful to repair the material defects of the TiO2 film. The optical characteristics of the TiO2 films were characterized by ellipsometry. It was found that the refractive index and the extinction coefficient of the TiO2 films increase with the annealing temperature. Further, the absorption coefficient was extracted and the rutile TiO2 film has the highest absorption coefficient among these samples. The deep level transient spectroscopy (DLTS) is used to extract the energy level and a number of the traps in the anatase-TiO2 film. Finally, the anatase, rutile, and mixed-phase TiO2-based metal-semiconductor-metal (MSM) photodetectors were fabricated. The Ni/Au was deposited on the TiO2 to form the Schottky junction. The Schottky-barrier heights between the Ni/Au and anatase, mixed-, and rutile TiO2 were extracted by current-voltage method. It was found that the Ni/Au on the rutile TiO2 film has the highest Schottky barrier height since the rutile TiO2 has less material defects which suppress Fermi level pinning. The cutoff wavelengths of the anatase-, mixed-, and rutile-TiO2 films are 380 nm, 385 nm, and 400 nm, respectively. The red shift of the cutoff wavelength results from the energy bandgap which became narrow from the anatase phase to the rutile phase. Further, the internal photoconductive gain is found in all MSM photodetectors. The anatase TiO2-based photodetector shows the highest photoresponsivity and detectivity of 3.34 A/W and 3.36×1012 Jones at 5 V. The rutile TiO2-based photodetector exhibits the lowest dark current of 6.06×10-10 A and the shortest response time.

Authors : Taejin Choi, Jeong-Gyu Song, Seunggi Seo, Seungmin Yeo, Hyungjun Kim; Byeonghyeon Jang, Soo-Hyun Kim;
Affiliations : Nanodevice Laboratory, School of Electrical and Electronic Engineering, Yonsei University, Seodaemun-Gu, Seoul 120-749, Republic of Korea; Nano-Devices and Process Laboratory, School of Materials Science and Engineering, Yeungnam University, Dae-Dong, Gyeongsan-Si 712-749, Republic of Korea;

Resume : Amorphous carbon (a-C) holds a particularly promising role in transparent conducting electrode, lubricating coating, secondary rechargeable battery electrode, and double patterning hardmask. Recently, the uniform and conformal a-C film coating on complex featured nanotemplates with the fine thickness control is a key issue for those emerging applications. Atomic layer deposition (ALD) has been considered as a promising technique to enable thin film deposition over large area uniformity, good conformality, and thickness control at the atomic-scale on high aspect-ratio nanostructures. Here we developed the plasma-enhanced ALD (PE-ALD) process of thin a-C film on a SiO2 substrate. Carbon tetrabromide (CBr4) is used as a precursor, and hydrogen plasma is used as a reactant. The saturated film growth rate is about 0.14 Α/cycle at the growth temperature of 300 °C. The a-C films consisted of nanocrystalline sp2 C and defective sp3 C incorporated with hydrogen and oxygen, and little bromine residue of 0.4 atomic % as detected in Raman spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy measurements. The in-situ surface hydroxylation and precursor exposure pretreatments prior to the a-C PE-ALD process are employed to enhance initial nucleation and smoothness of a-C thin film deposition. Also, conformal growth of a-C thin films on three-dimensional (3-D) structures was confirmed. The electrical properties of our a-C films were comparable with other reported a-C films.

Authors : M. Pelletta, P. Siffalovic, M. Hodas*, Y. Halahovets, K. Vegso**, M. Jergel, E. Majkova
Affiliations : Institute of Physics, Slovak Academy of Sciences, Dubravska cesta 9, 845 11 Bratislava, Slovakia; *Institute of Applied Physics, University of Tubingen, 72076 Tubingen, Germany; **Japan Synchrotron Radiation Research Institute, 1-1-1, Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 Japan

Resume : Copper is a standard material for fabrication of conductive contacts on 2D-materials including graphene. Even though copper exhibits the Volmer-Weber growth mode on both graphene and graphite, characterized by the formation of 3D islands, considerable differences in the growth kinetics may arise from different copper adatom adsorption and diffusion energies. Herein we present a unique laboratory-based grazing-incidence small-angle X-ray scattering (GISAXS) technique which allows to track the temporal evolution of the copper thin film growth on graphene surface. We studied the influence of the substrate temperature. In all GISAXS datasets collected at various temperatures, it is possible to recognize three main growth stages, namely nucleation and cluster growth, dynamic coalescence and early stage of percolation. The nucleation density of 3.4x10^12 cm^-2 at T=323K decreases down to 4.8x10^11 cm^-2 at T=373K due to the enhanced mobility of copper adatoms on graphene. The power law scaling constant for the coalescence stage increases with the substrate temperature, being in good agreement with the results published for other weakly interacting surfaces. The experimental results achieved show the importance of in-situ GISAXS studies for a real-time growth monitoring of copper and other noble metals on graphene.

Authors : A. Lomov, K. Shcherbachev, Yu. Chesnokov, A. Miakonkikh, D. Kiselev
Affiliations : Institute of Physics and Technology of Russian Academy of Sciences, Moscow, Russia; National University of Science and Technology MISiS, Moscow, Russia; National Research Centre “Kurchatov Institute”, Moscow, Russia; Institute of Physics and Technology of Russian Academy of Sciences, Moscow, Russia; National University of Science and Technology MISiS, Moscow, Russia

Resume : Creation of semiconductor materials with advanced physical properties and engineering of shallow junctions and strained layers with a depth of less than several tens of nm are the main trends for ultra-large scale integration circuits (ULSI). Nowadays this intention can be realized by forming nanoscale silicon layers in a different phase state by high dose Plasma-immersion ion implantation (PIII) with low energies (0.5-5keV). For modification of structural and electrical properties of semiconductor substrates noble gas ions are very promising. Unfortunately crystal lattice damages and structural defects created during implantation and subsequent annealing change physical properties of such layers. Metrological control of low-dimension multilayers both fabrication and post technological treatment is required. In this work we investigated structural changes of He+ PIII implanted silicon layers after implantation and subsequent thermal annealing. Samples 20 × 20 mm in size were cut out from p-type (= 12 Ω cm ) Cz-Si(001) wafer. The high-dose (D = 5×1017 cm–2) implantation of He+ ions was performed at room temperature by applying 10-μs rectangular pulses of negative accelerating potential (2 or 5 kV) with a frequency of 1 kHz in a plasma-immersion low-voltage ion implanter (FTIAN RAN), equipped with an inductively coupled plasma source. After implantation the samples were annealed in vacuum at 580 and 800С for 30 min. To characterize structural evolution of the layers high-resolution X-ray reflectivity (HRXRR), diffraction (HRXRD), transmission electron microscopy (TEM), Rutherford backscattering spectroscopy (RBS), and atomic force microscopy (AFM) methods were used. Formation of a three-layer structure (amorphous a-SiOx layer at the surface, amorphous a-Si layer with helium bubbles and buried helium bubbles heavy damaged tensile strained crystalline c-Si layer) that is retained after annealing was observed. Helium-filled bubbles are observed in an as-implanted sample. Evolution of the multilayer structure and the bubbles due to annealing are revealed and comparing with the structural parameters of an as-implanted sample was done. The bubbles are shown to trend into bimodal distribution after annealing. The characteristic bubble size is determined to be in a range of 2–20 nm. Large size helium-filled bubbles are located in the amorphous a-Si layer. Small size bubbles are revealed inside the damaged crystalline Si layer. These bubbles are a major source of tensile strain in c-Si layer. Comparison of XRR, HRXRD and RBS results showed that the helium filled bubbles located in low-density sublayer at the depth of about Rp is a major source of the tensile strain in the damaged layer. The characteristic bubble size is estimated to be 2–20 nm. The middle bubble size is smaller for low energy implanted sample, what may be explained by remarkable surface influence. The value of tensile strain is a function of PIII and annealing regimes. It was shown that application of these complementary methods allows one to reveal crystal structure evolution of Si surface layers after low-energy high-dose He+ implantation and subsequent annealing.

Characterization methods at the nanoscale of nano-engineered thin films 1 : F. Vaz + M. Lavisse
Authors : Jurriaan Schmitz
Affiliations : MESA Institute for Nanotechnology, University of Twente, Enschede, The Netherlands

Resume : In the area of microelectronics, a recent trend is the rapid introduction of new thin-film materials. There is a need for higher-performant materials at ever smaller dimensions; but also more practical aspects such as the step coverage and film uniformity can be decisive for the replacement of one material with another. A central concern for all thin films in microelectronics is the deposition of high-quality (and stable) layers at relatively low temperatures. Atomic layer deposition technology [1,2] can offer a combination of relatively low temperatures (compared to chemical vapor deposition, the industry standard for thin films in microelectronics) with high step coverage and good thickness control and uniformity. Using atomic layer deposition, two-atomic materials are most commonly deposited. Well studied ALD materials are Al2O3, HfO2 and TiN. A concern for ALD is that a dedicated process needs to be developed for each material. The repetitive use of two (or sometimes more) precursors, separated in time or space, requires a process window where the precursors react with the substrate in a self-limiting manner at the same substrate temperature. In spite of this, ALD has become the process of choice for a host of materials in microelectronic chip fabrication. Studies of TiN deposition on thermally grown SiO2 in our group, using thermal ALD, have shown that the first layers of this material form according to the Stranski-Krastanov process. We have investigated the optical and electrical properties of the deposited TiN in detail, in the thickness range from 0.65 to 20 nm [3]. We obtained a remarkably strong field effect in subnanometer TiN films. The film resistivity was modulated by as much as 17% by an external field [4], whereas earlier reports of the field effect in metals mention 10-6 or lower relative resistance change. The oxidation of the TiN film, which occurs at relatively low temperatures [5], must be prevented by a capping layer. The use of a plasma can expand the possibilities of ALD [6-8]. The plasma provides radicals rather than stable molecules and therefore allows surface reactions to take place at lower substrate temperatures. Furthermore, it can open the possibility to deposit materials for which no thermal ALD process window exists with given precursors. Examples include elemental metals such as Pt and Pd. We do see a decrease of the step coverage performance as well as reduced layer uniformity when plasmas are employed in ALD. Recent work in our group aims to mitigate this disadvantage of plasma-enhanced ALD by new reactor concepts, in which radicals are supplied to the wafer surface without the involvement of a plasma. In particular we have shown that the dissociation of precursor molecules using a tungsten hot wire provides a relatively clean source of radicals. With these radicals, new materials can be grown using ALD. Examples in this presentation will include tungsten and aluminum nitride. Tungsten (W) thin films were grown using hot wire ALD with H2 and WF6 precursors [9]. The hot wire was used to generate atomic hydrogen, which is subsequently used to remove the fluorine from the surface after a (self-limiting) WF6 exposure. We found a means to deposit either α-W or β-W, two polycrystalline states with different resistivity, using this equipment, by a controlled change of deposition conditions. Aluminum nitride is commonly deposited by sputtering. We investigate AlN deposition using thermal or radical-assisted ALD to provide conformal thin films with a thickness in the range of a few tens of nanometers [10]. The depositions are based on TMA/NH3 chemistry. When the ammonia is led along the hot wire, it decomposes to form nitrogen-containing radicals. This significantly lowers the minimum temperature for the growth of good-quality films; but is also found to impact the material structure and composition. The supply of precursor radicals using other means than plasma has shown to provide additional experimental freedom and allows to deposit materials with better properties than before. This enables the introduction of new, better performing materials in next-generation microchips in line with the international roadmap for semiconductor technology. References: [1] S. M. George, Chem. Rev. 2010, 110, 111. [2] B. S. Lim, A. Rahtu, R. Y. G. Gordon, Nature Materials 2003, 2, 749. [3] H. Van Bui, A. Y. Kovalgin and R. A. M. Wolters, Applied Surface Science 269 (2013) 45-49. [4] H. Van Bui, A. Y. Kovalgin, R. A. M. Wolters and J. Schmitz, Appl. Phys. Lett. 103, 051904 (2013). [5] H. Van Bui, A. W. Groenland, A. A. I. Aarnink, R. A. M. Wolters, J. Schmitz and A. Y. Kovalgin, J. Electrochem. Soc. 158 (3) H214-220 (2011). [6] Y. J. Lee, S.-W. Kang, Electrochem. and Solid-State Let. 2002, 5, C91. [7] Y. J. Lee, S.-W. Kang, Thin Solid Films 2004, 446, 227. [8] C. Ozgit, I. Donmez, M. Alevli, N. Biyikli, J. Vac. Sci. Technol. A, 2012, 30, 01A124. [9] M. Yang, A. A. Aarnink, A. Y. Kovalgin, D. J. Gravesteijn, R. A. Wolters, J. Schmitz, J. Vac. Sci. Technol. A, 2016, 34, 01A129. [10] A. Y. Kovalgin et al., Hot-wire assisted ALD: a study powered by in-situ Spectroscopic Ellipsometry, manuscript submitted to Advanced Materials Interfaces (2017).

Authors : René Hammer*, Jozef Keckes**, Juraj Todt**, Bernhard Sartory*, Jochen Kraft***, and Stefan Defregger*
Affiliations : *Materials Center Leoben Forschung GmbH, Roseggerstraße 12, 8700 Leoben, Austria **Montanuniversität Leoben, Franz-Josef-Straße 18, 8700 Leoben, Austria ***AMS AG, Tobelbader Strasse 30, 8141 Unterpremstätten, Austria

Resume : For reliability in microelectronics residual stress is of major concern, because it can reach the giga-Pascal range in thin films. It acts as a driving force for failure modes like fracture and delamination. The difference of the stress averaged by film thickness and the maximum stress peaks can be significant. For this reason a method which is able to reveal a local depth resolved stress profile is desired. In this study micro-cantilevers are fabricated from CVD W thin films on silicon substrates by ion slicing and focused ion beam. Using the ion beam layer removal (ILR) method [1] slices of ~10nm depth resolution are removed from the film and the depth resolved residual stress profile is computed. Wafer curvature measurements show an overall mean stress in the W layer of around 1 GPa. On the other hand the maximal stress in W, measured with ILR, is up to 6 GPa. This is greatly exceeding the flow stress of microcrystalline W which is ~0.6 GPa. The obtained stress profile can be described well by correlation with the grain size distribution, obtained by EBSD measurements, using a Hall-Petch relationship for grain boundary strengthening [2]. The findings suggest that the use grain-size control in W is an important tool when residual stress engineering is desired. [1] R. Schöngrundner, R. Treml, T. Antretter, D. Kozic, W. Ecker, D. Kiener and R. Brunner, Critical assessment of the determination of residual stress profiles in thin films by means of the ion beam layer removal method, Thin Solid Films 564, pp. 321-330, 2014. [2] R. Hammer, J. Keckes, J. Todt, B. Sartory, J. Kraft, and S. Defregger, Depth-resolved residual stress measurement in W-TiN thin films: revealing Hall-Petch-related stress profile, to be submitted to Materials & Design.

Authors : J.J. Colin, A. Michel, C. Furgeaud, C. Mastail, G. Abadias
Affiliations : Institut Pprime, UPR 3346 CNRS-Université de Poitiers-ENSMA, Département de Physique et Mécanique des Matériaux, SP2MI, Bld Marie et Pierre Curie, Téléport 2, 86962 Chasseneuil, France

Resume : Metal silicides, key building-blocks of continuously miniaturised Si-based integrated circuits, necessitate control of the interfacial silicide reaction during deposition of nanoscale metal films, although the dynamic processes involved remain obscure to date. Pd films were deposited by magnetron sputtering on Si(001) covered by native oxide, amorphous Si (a-Si) or Ge (a-Ge) buffer. The effects of substrate temperature during growth (T < 250°C) are also discussed. The film growth was investigated by in situ and real-time stress measurements (MOSS), in-situ resistivity measurements, and ex-situ structural characterisation (XRD, AFM, TEM, EELS). Initial growth stages follow a 3D mode. In the case of a-Si, an interfacial reaction results in a 2D growth mode; the resulting amorphous silicide upon increasing deposition thickness (>2 nm) transforms into the crystalline hexagonal Pd2Si phase, with an associated tensile stress. Eventually, a (111)-textured Pd film is obtained under compressive stress signature consistent with defect incorporation during energetic conditions growth. At higher temperatures, the competition between interfacial silicide reaction and Pd growth results in extremely complex stress changes; these can be explained by considering the a-Si layer as a limited Si reservoir for silicide formation. In all cases, concurrent diffusion of Pd and Si atoms highlight the importance of grain boundaries and thus the energetic and kinetic conditions during growth.

Authors : Peter Firth, Zachary Holman
Affiliations : Arizona State University;Swift Coat

Resume : Many applications that utilize nanomaterials in manufactured products require that the particles be deposited as films or coatings. These may be, for example, thermal barrier coatings on high-temperature parts, active layers in electronic devices, optical layers in laser Bragg mirrors, or biocompatible coatings for medical applications. In all cases, theses coatings should be able to be deposited rapidly over large areas, have a uniform and controllable thickness, and their constituent particles should maintain their unique nano-scale properties. Present nanomaterial films developed in laboratories are often unable to be reproduced on an industrial scale; the manufacturing methods are inherently nanomaterial and substrate specific. This specificity results in manufacturing equipment that is expensive or offers limited utility. We propose an advanced nanomaterial film manufacturing technology based on hypersonic particle deposition (HPD) that overcomes these deficiencies. HPD begins by aerosolizing a nanomaterial using any desired technique, from atomizing a nanoparticle-laden solution to feeding nanoparticle-precursor gas into a plasma. The aerosolized material is fed into the HPD system, which consists of two chambers separated by a slit-shaped nozzle, with the bottom chamber held under vacuum (0.01¬–1 Torr). The nanomaterial is accelerated to a velocity of several hundred meters/second as it and the aerosol background gas are forced through the nozzle, resulting in the formation of a curtain of nanoparticles directed into the downstream chamber. A substrate is passed through the curtain, and the nanomaterial collides with and adheres to the substrate, forming a thin coating. Utilizing plasma synthesized silicon nanoparticles, we will showcase a custom designed HPD system capable of forming uniform thin films of controllable thickness and porosity on substrates up to 130 mm by 130 mm. Through a combination of scanning electron microscopy, Rutherford backscattering and elliposometry we demonstrate silicon nanoparticle films with independently tunable thicknesses between 50 nm and 3 μm and porosities between 67% and 95%. We further demonstrate the scalability of this process by forming films with <7.5% thickness non-uniformity and <1% porosity non-uniformity on 130 mm silicon substrates.

Authors : Khac Bien Cuong Tran, Koo-Hyun Chung
Affiliations : School of Mechanical Engineering, University of Ulsan, Ulsan 680-749, South Korea.

Resume : The layered materials, such as hexagonal boron nitride (h-BN), molybdenum disulfide (MoS2) and graphene have been recently proposed as protective coating layers for micro- and nano-devices due to their low friction characteristics, remarkable mechanical properties, and chemical inertness. Extensive efforts have been devoted to understand the tribological characteristics of these materials. In particular, friction of the layered materials was found to increase as the number of layers decreased. However, in contrast to friction characteristics, surface damage characteristics remain relatively unexplored. In this work, the surface damage characteristics of single- and few-layer h-BN, MoS2, and graphene were systematically assessed using atomic force microscopy (AFM) and Raman spectroscopy. In details, AFM-based progressive and constant force scratch tests were performed on the h-BN, MoS2, and graphene flakes deposited on Si/SiO2 substrate by mechanical exfoliation. AFM topographic images and Raman spectra were then obtained to understand the surface damages characteristics of the flakes. The results showed that graphene exhibited higher surface damage resistance than MoS2 and h-BN. It was also found that the surface damage characteristics may differ depending on the number of layers. The outcomes of this work may be helpful to elucidate the feasibility of single- and few-layer h-BN, MoS2, and graphene as a protective coating layer for micro- and nano-devices.

Poster session 1: Preparation, Characterization and Properties of Thin Films : F. Vaz + T. Polcar
Authors : Saâd Rahmane, Benchiha kheira, Allag Abdelkrim, Attouche Hafida and Kouidri Nabila
Affiliations : Laboratoire de Physique des couches minces et applications, Université de Biskra, BP 145 RP, 07000 Biskra, Algérie

Resume : In this work, aluminium-doped zinc oxide thin films (ZnO:Al) have been produced by spray pyrolysis and magnetron sputtering methods. All the films prepared by spray pyrolysis were uniform and well adherent to the substrates, XRD studies showed that the films grow with (002) preferred orientation. Estimated band gap energy from optical absorption data is from 3.2 to 3.4 eV. The measured electrical conductivity at room temperature was found in the order of 10-1(.cm)-1 for ZnO and it is higher by two order of magnitude for ZnO:Al. For films prepared by magnetron sputtering, we observed that, with increasing rf power the growth rate increased, while it decreased with increasing gas pressure. As mentioned above, the films were polycrystalline in nature with a strong preferred (002) orientation. The intrinsic compressive stress was found to decrease with both increasing rf power and gas pressure, and near stress-free film was obtained at 200 W rf power and 2x10-3 mbar gas pressure. The obtained ZnO:Al films, not only have an average transmittance greater than 90 % in the visible region, but also have an optical band gap between 3.33 and 3.47 eV depending on the sputtering parameters. Moreover, a low value of the electrical resistivity (~1.25x10-3 Ωcm) was obtained for the film deposited at 200 W and 2x10-3 mbar. From these results it is concluded that the home made spray pyrolysis system is suitable technique for obtaining thin films of ZnO:Al with good properties compared to the films obtained by sputtering magnetron technique. Further optimisation of spray system is still in progress in order to improve the crystalline quality of the films and increase their electrical conductivity.

Authors : Han-Ki Kim1 and Tae-Woong Kim2
Affiliations : 1Kyung Hee University, Department of Advanced Materials Engineering for Information and Electronics, 1 Seocheon, Yongin, Gyeonggi-do 446-701, Republic of Korea 2Samsung Display, OLED R&D Center, Yongin, Gyeonggi-do 446-711, Republic of Korea

Resume : Asymmetric flexible ZTO/Ag/ITO and ITO/Ag/ZTO multilayers were sputtered onto flexible PET substrate by using a lab scale roll-to-roll (RTR) sputtering system to use as a flexible and transparent anode for flexible organic light emitting diodes (OLEDs). To optimize the electrical and optical properties of the asymmetric ZTO/Ag/ITO and ITO/Ag/ZTO multilayer, the thickness of Ag interlayer were varied by controlling of the DC power applied on Ag target during the RTR sputtering process. At an optimized thickness of Ag, the asymmetric ITO/Ag(10 nm)/ZTO/PET and ZTO/Ag(12)/ITO/PET sample showed the highest figure of merit value due to low sheet resistance and high optical transmittance. In addition, surface morphology and mechanical flexibility of the asymmetric ZTO/Ag/ITO and ITO/Ag/ZTO multilayer were investigated as a function of the Ag interlayer thickness. Various bending test results showed that both ZTO/Ag/ITO and ITO/Ag/ZTO multilayer had a good flexibility due to high strain failure of Ag interlayer, which is acceptable in fabrication of flexible OLEDs. Although both asymmetric ZTO/Ag/ITO and ITO/Ag/ZTO multilayer showed similar sheet resistance and optical transmittance, the flexible OLED fabricated on each ZTO/Ag/ITO and ITO/Ag/ZTO anode showed different performance due to different work function of top oxide layer. Better current density-voltage-luminance characteristics of the flexible OLED on the ITO/Ag/ZTO/PET than that of flexible OLED on ZTO/Ag/ITO/PET indicates that the top transparent oxide with high work function is favorable in asymmetric oxide-metal-oxide multilayer for high performance flexible OLEDs.

Authors : Jung-Dae Kwon, Se-Hun Kwon, and Jin-Seong Park.
Affiliations : Korea Institute of Materials Science, Pusan National University, and Hanyang University

Resume : Copper oxide(CuOx) films were grown at a relatively low temperature (100 °C) by atomic layer deposition (ALD). Hexafluoroacetyl-acetonate Cu(I) (3,3-Dimethyl-1-butene) ((hfac)Cu-(I)(DMB)) and ozone (O3) were used as the copper precursor and oxidant, respectively. It is shown that stable phases of CuOx are obtained through rapid thermal annealing (RTA) in air. After annealing at various temperatures (200~ 500°C), different p-type band structures and electron binding information are obtained. X-ray photoelectron spectroscopy (XPS) and spectroscopic ellipsometry (SE) studies indicate that the major copper oxidation state changes from 1+ to 2+ during thermal treatment. Thin film transistors (TFTs) incorporating the ALD-grown CuOx semiconductors are evaluated, and an unusually high p-type device performance is observed, with a field effect mobility of 5.6 cm2/Vs after annealing at 300°C.

Authors : Joonam Kim, Ken-ichi Haga, Eisuke Tokumitsu
Affiliations : School of Materials Science, Japan Advanced Institute of Science and Technology

Resume : MoS2, one of the two dimensional dichalcogenide materials, has attracted much attention as a new semiconductor for future electrics applications. To fabricate MoS2 thin films, the mechanical exfoliation method and the chemical vapor deposition are commonly used, but there are only a few reports on the chemical solution process. In this work, we report coating properties of chemical solution processed MoS2 thin films on various kinds of oxide materials. The source solution of 0.1 M ammonium tetrathiomolybdate ((NH4)2MoS4) dissolved in n-methyl-2-pyrrolidone (NMP) was spin-coated on SiO2, Al2O3, HfO2, ZrO2, Pb(Zr,Ti)O3, and (Bi,La)4Ti3O12. Poor coating properties were observed for SiO2 and Pb(Zr,Ti)O3 whereas good coating properties for the other oxides. This can be understood by the surface energies of the oxide, using the van Oss-Chauhury-Good theory. It is shown that the oxide with large electron-acceptor parameter results in poor coating property. Next, to form the MoS2 film, the spin-coated film was annealed at 400C in H2/Ar (5:95) atmosphere for 30 min, followed by 1000C annealing in Ar atmosphere with sulfur vapor for crystallization. We confirmed by Raman spectroscopy and transmission electron microscope (TEM) observation that the two-dimensional MoS2 crystallized film was grown on ZrO2, following the surface roughness of the substrate in several tens of nm. Hence, the chemical solution process is one the promising techniques for MoS2 film formation.

Authors : S.B. Donaev, B.E. Umirzakov, D.A.Tashmukhamedova
Affiliations : Tashkent state technical university

Resume : Electrovacuum devices, its characteristics do not yet have equivalent analogues among the new types of semiconductor and microelectronic devices. But making ultrahigh frequency devices with the necessary performance and a high degree of reliability is still an unsolved problem. The relevance of these investigations to the development of nanotechnology has increased significantly. The electronic devices as cathodes are widely used alloyed cathodes type of Pt-Ba, Pd-Ba. Thereby important problems are the increase in emission efficiency, stability, elimination of high-temperature heating. The possibility of replacing the precious metals with other materials significantly reduces the cost and size of the device. In the case of secondary emission ("cold") cathodes the most effective materials for them were the Pt-Ba and Pd-Ba, activated in an atmosphere of H2 and N2. In some cases, the coefficient of secondary electron emission m increased from 4 to 6. However, the simple exposure of these cathodes even in a vacuum of 10-6 mm Hg m leads to a decrease to 2.8 - 3. These problems require innovative approaches to its solution. One possible approach is to improve the cathodes based on metals and alloys by means of ion implantation in combination with various types of annealing (thermal, laser and electron bombardment). The use of ion implantation can increase the value KVEE m 3 times or more, in some cases, instead of Pt and Pd can be used Mo and W. If you need to re-Activation of, it can be carried out by laser irradiation. The report presents the main features of the use of ion implantation for obtaining nanoscale structures leading to improved emission efficiency and lifetime of alloy cathodes PdBa and PtBa.

Authors : Woo Seok Kang, Min Hur, Jae-Ok Lee, Young-Hoon Song
Affiliations : Korea Institute of Machinery & Materials

Resume : Atmospheric-pressure plasma process is a cost-effective manufacturing way of thin-film deposition without requiring complex vacuum auxiliary systems. Here we report a novel dielectric barrier discharge (DBD) reactor for plasma processes of functional treatment and thin-film coatings under atmospheric pressure. Optical and electrical measurement shows that the developed reactor, which is consisted with two back-to-back L-shaped electrodes driven by bipolar voltage pulses, generates spatially homogeneous stable plasmas. After functional treatment by using the developed reactor, a polymer (polyimide) surface becomes more hydrophilic with enhanced adhesive characteristics. The unique electrode geometry of the developed reactor enables to control the generation of reactive species for the effective plasma treatment sustaining stable homogeneous mode. For atmospheric-pressure PECVD, several process steps were developed to demonstrate the zirconium dioxide (ZrO2) thin film deposition. Plasma stability and the quality of the ZrO2 layer were strongly affected by the counterbalance between oxygen and precursor, tetrakis(ethylmethylamido)zirconium (TEMAZr), during the deposition process. We found that controlling the gas/precursor flow stream is critical to achieve uniform layers during atmospheric-pressure PECVD processes. Finally, feasibility of extending the current small lab-scale reactor to wide-area one for the industrial use will be discussed.

Authors : Quentin Hatte, Samuel Branchu, Pierre Antoine Dubos, Mireille Richard-Plouet, Pascal Casari, Pierre Yves Jouan
Affiliations : IRT Jules Verne, Chemin du Chaffault, 44340 Bouguenais ; Institut de recherche en génie civil et mécanique, UMR6183, IUT de Saint-Nazaire, 58 rue Michel Ange, BP 420 - 44606 Saint Nazaire Cedex ; Institut de recherche en génie civil et mécanique, UMR6183, IUT de Saint-Nazaire, 58 rue Michel Ange, BP 420 - 44606 Saint Nazaire Cedex ; Institut des Matériaux Jean Rouxel, CNRS UMR6502, 2 rue de la Houssinière – BP 32229 44322 Nantes cedex 3 ; Institut de recherche en génie civil et mécanique, UMR6183, IUT de Saint-Nazaire, 58 rue Michel Ange, BP 420 - 44606 Saint Nazaire Cedex ; Institut des Matériaux Jean Rouxel, CNRS UMR6502, 2 rue de la Houssinière – BP 32229 44322 Nantes cedex 3

Resume : Wind and hydraulic devices are most generally located in challenging operating environments such as corrosive atmospheres. Durability of coatings is an important issue in order to limit maintenance that may be expensive since the lifetime of these infrastructures can reach 25 years. This study, part of the OPTISURF project aims at testing, improving and combining several surface treatments. One of the considered solutions is to deposit a first layer of metal and metal oxide coatings on steel substrate by PVD (Physical Vapor Deposition) HiPIMS (High Power Impulsed Magnetron Sputtering). These coatings are tested as a surface treatment before industrial painting systems. Previous works have shown that Nickel and Nickel oxide coating presents good corrosion resistance properties on XC38 steel substrate [1]. A good knowledge of microstructural and mechanical properties helps to improve the efficiency of coatings against corrosion. The performance evaluations are conducted on thin films deposited on S355 steel substrate which is commonly used. Several characterization techniques are carried out, such as, energy dispersive X-ray analysis coupled with scanning electron microscopy, microhardness, neutral salt spray resistance and adhesion tests. First results show better corrosion resistance and adhesion properties of the global system with the deposition of the PVD layer at the surface of the steel substrate, before the paint. [1] J. Keraudy, PhD thesis, University of Nantes, 2015.

Authors : Quyet Van Le, Ju Hyun Jeon, Soo Young Kim
Affiliations : Chung-Ang University; Chung-Ang University; Chung-Ang University

Resume : In recent year, organic/inorganic metallic halides have emerged as a new class of materials for optoelectronic device such as solar cells, light emitting diodes, and lasers. In this report, methylamine lead halides were grown by two step deposition using lead (II) acetate trihydrate (Pb(CH3CO2)2.3H2O) and methyl amine halide (CH3NH3X, X: Cl, Br, and I). By controlling the synthetic condition such as concentration of precursor and annealing temperature, the methylamine lead halides can be synthesized with various structures such as nanocube, nanowire, nanorod, shrinkage-induce film, and rod on shrinkage-induce film. The change of methylamine lead halides’ shapes makes it possible to control the surface contact area, electrical and optical properties, which are important factors for optimize the device performance. The characteristics of methylamine lead halides were fully investigated using scanning electron microscopy, UV-vis absorbance, photoluminescence spectroscopy, synchrotron radiation spectroscopy, and ultraviolet photoelectron spectroscopy. The applications of methylamine lead halides to optoelectronic have been investigated and discussed. ACKNOWLEDGEMENT This research was supported in part by a National Research Foundation of Korea (NRF) grant funded by the Korean government (MSIP) (No. 2014R1A2A1A11051098, 2015K1A3A1A59073839).

Authors : 1Youngwoo Jeong, 2Soonho Park, 2Jaehyoung Park, 3Taewook Kang, 4Heelack Choi, 5Taehoon Kim, 2, 3*Jongsu Kim
Affiliations : 1Department of LED Convergence Engineering, Pukyong National University, Busan, 608-737, South Korea 2 Department of Display science & engnieering, Pukyoung National University, Busan, 608-737, South Korea 3 Interdisciplinary Program of LED and Solid State Lighting Engineering, Pukyong National University, Busan, 608-739, South Korea 4 Department of material science and engineering, Pukyoung National University, Busan, 608-737, South Korea 5 87, Gunjacheon-ro 21beon-gil, Siheung-si, Gyeonggi-do, Korea

Resume : Blue-to-UVC upconversion of Y2Si2O7:Pr3+ phosphor film was demonstrated. The film was coated on the quartz substrate with Y-Si-Pr stoichiometric-contained solution, and then annealed at high temperature in a vacuum atmosphere. The obtained film showed the triclinic structure of Y2Si2O7:Pr3+ phosphor. It showed the sharp Pr3+-based f-f transitional downconversion spectrum with dominant peaks at 477 nm and 610 nm as well as the broad Pr3+-based f-d transitional downconversion spectrum with a main peaks at 270 nm by a higher-energy excitation. Some surface cracks was minimized through slower cooling, and the optimized film showed the crack-free surface morphology and the thickness of about 800 nm. The phosphor film showed strong UVC emission with a main peak of 270 nm by a lower-energy light in the blue region, which is coincident with the germicidal curve. The surface pattern of the phosphor film and the shape of the quartz substrate was optimized on the base with LightTools simulation to minimize the internal reflections of UVC emission. Finally, the sterilization of microalgae was demonstrated by the UVC upconversion phosphor under an excitation of 465 nm blue LEDs.

Authors : Ho Young Jun, Eon Ju Lee, Si Ok Ryu*
Affiliations : School of Chemical Engineering, Yeungnam University, 280 Daehak-ro, Gyeongsan 712-749, South Korea

Resume : Black phosphorus (BP), the most stable allotrope of phosphorus, is a material stacking individual atomic layers together through van der Walls interactions. Bulk BP has a structure similar to graphite and is the only elemental substance that can be mechanically exfoliated into an ultra-thin nanosheet other than graphite. In recent studies, the band gap of BP is tunable from 0.3eV for bulk BP to 2.0eV for phosphorene (monolayer BP) depending on the number of stacked layers. In this work, two-dimensional black phosphorus (phosphorene) dispersed in a solution is obtained by the solvent exfoliation. Among various solvents, N-methylpyrrolidone (NMP) is found to provide stable, highly concentrated BP dispersions. In addition, black phosphorous thin films were also deposited on the substrates using ink-jet printing method. Physical properties of the films were systematically characterized by atomic force microscope (AFM), scanning electron microscopy (SEM) and Raman spectroscopy. The electrical characteristics of TFTs fabricated with the deposited films were investigated by a three-probe station. In this study, the stable, highly concentrated, electronic-grade phosphorous thin films were successfully deposited by combining the solvent exfoliation with the ink-jet printing deposition method. Considering our result obtained in this study, it is believed that the black phosphorene prepared in this study could be applied to large-area, high-performance phosphorene devices.

Authors : 1 R.K.Savkina, A.B. Smirnov, A. I. Gudymenko, V. P. Kladko, A. A. Korchovyi, A. S. Nikolenko, M.I. Smoliy, V. V. Strelchuk 2 T.G.Кryshtab
Affiliations : 1 V.Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine, 41 Nauky av, Kyiv 03028, Ukraine; 2 Instituto Politécnico Nacional - ESFM, Department of Physics, Av. IPN, Ed. 9 U.P.A.L.M., 07738, Mexico D.F.

Resume : Extreme conditions of the ultrasonic cavitation such as local temperature and pressure are widely used in chemistry, as for example to synthesize nano-materials, to enhance the electrochemical reactions and to modify the surface properties of electrodes. The ultrasonic irradiation is a powerful tool in promoting of the chemical reactivity in the liquids at solid surfaces also. In our experiments described here, the application of ultrasonic approach for the modification of silicon surface is summarized. The properties of the silicon samples subjected to cavitation impacts have been studied. Boron-doped p-type (100) silicon (wafers grown by the liquid-encapsulated Czochralski method, with diameter about 76.2-mm) were used in this study. It was shown that high-intensity (15 W/cm2) and high-frequency (1 ÷ 6 MHz) sonication of silicon samples in the liquid nitrogen induces changes of the physical, chemical, and structural properties of semiconductor surface. Optical, atomic force and scanning electron microscopy techniques as well as energy dispersive X-ray spectroscopy, µ-Raman spectroscopy and HRXRD measurements were used. Using the ultrasonic cavitation to manipulate semiconductor surfaces on a small scale allowed us to obtain silicon with a unique combination of photovoltaic and photoluminescent properties as well as with biocompatible material (calcium silicate) on the surface.

Affiliations : Department of Physics, Istanbul Technical University

Resume : Among transparent conducting oxides (TCOs), indium-doped tin oxide (ITO) is the most widely used material as a key component for a wide range of electronic and opto-electronic devices, including solar cells, gas sensors, light-emitting diodes (LEDs), thin film transistors, and photodetectors due to its unique combination of electrical and optical properties. Despite its perfect electrical and optical properties as a TCO material, the scarcity of indium limits the extensive use of ITO for device applications at large-scale. In this regard, ZnO has been considered as a potential candidate to replace ITO. ZnO is a wide-band gap semiconductor (3,37 eV) with a high exciton binding energy (60 meV) at room temperature. It is known that despite its high transparency in the visible region, intrinsic-ZnO is a high resistive material. In order to effectively enhance its properties, ZnO is doped with selective elements, such as Al, Ga, In and Sn. Among them, Sn is particularly appropriate dopant due to the ease of replacing Zn in the lattice structure, stemming from the known small radius difference between the two atoms (r Zn=0,074nm, r Sn=0,069nm). In this study, undoped and Sn doped ZnO thin films with different Sn concentrations were successfully deposited on soda-lime glass substrates using RF/DC sputtering technique. The effects of Sn doping concentration and annealing on structural, electrical, and optical properties of Sn doped ZnO thin films, between 0.5 and 3 %, was determined in detail. The crystal structure of undoped and Sn doped ZnO thin films were analyzed by XRD measurements, which revealed the preferential orientation along the (002) plane for the all the films and the deterioration of crystallinity as well as a gradual shift of main peak position to higher values following the doping process. Following the annealing process, between 150oC and 500oC, a drastic improvement in crystallinity of both doped and undoped ZnO films was observed. AFM measurements have shown that there is a significant modification in surface morphology following the doping process. The transmission measurements indicated an average transmittance of 90 % in the visible range for the doped films annealed at 500oC under N2 gas flow. From the transmission and reflection measurements it was observed that there is a gradual decrease in band gap with an increase in doping concentration, which means the band gap shrinkage following the doping process. In addition to this, it was revealed that there is an increase in band gap with increase of annealing temperature. The room temperature electrical resistivity of the doped films was measured by four-point probe and the lowest resistivity, 9.8x10-3Ωcm, was measured for 1.5% Sn-doped ZnO thin film following the post-annealing process at 250oC.

Authors : Hamed Behzad Farhad E Ghodsi Elif Peksu Hakan Karaagac
Affiliations : Department of Physics, Faculty of Science, The University of Guilan, Namjoo Avenue, 413351914 Rasht, Iran Department of Physics Engineering , Istanbul Technical University, Maslak, 34469 Istanbul, Turkey

Resume : In this study, copper- doped cobalt-oxide thin films (CuxCo3-xO4, 0 ≤ x ≤ 1.25) have been successfully deposited on soda-lime glass substrates using sol-gel technique. The effect of Cu content on the crystalline structure of the deposited thin films was determined via grazing incident X-ray diffraction (GIXRD) patterns, which revealed a decrease in crystallinity following the gradual increase in Cu concentration as well as the coexistence of a secondary phase (CuO) and spinel CuCo2O4 phase for x ≥0.75. The effect of Cu content on the localized states in the energy gap, known has a significant effect on determining the performance of a wide range of this material based electronic and opto-electronic devices, including solar cells and photo-catalysts, was investigated by calculating the Urbach energy from transmittance and reflectance measurements. The results have shown that the incorporation of Cu ions into Co3O4 structure leads to an increase in Urbach energy, deduced from the observed increase in the disorder of the lattice, and a decrease in the concentration of localized states in the forbidden band gap region with further increase in Cu concentration, which was attributed to the formation of inverse spinel structure at higher Cu-concentrations. As a final part of this study, detailed analyses of chemical composition of the films was carried out by X-ray photoelectron spectroscopy (XPS) measurements. The XPS depth profiling measurements have shown that for x ≥1, extra Cu atoms leave CuCo2O4 spinel structure so as to form CuO layer on top of the deposited films.

Authors : Daniel Javdošňák, Jindřich Musil, Radomír Čerstvý, Stanislav Haviár, G. Remnev, V. Uglov
Affiliations : University of West Bohemia, Univerzitní 8, 306 14 Plzeň, Czech Republic

Resume : The Al-Si-N thin films with a low Si content (<5 at.%) were deposited by ac pulsed (unipolar) reactive magnetron sputtering. The structure, microstructure, mechanical and optical properties of the Al-Si-N films are analyzed in detail. The effect of the energy delivered Ebi in the growing film by bombarding ions on the properties of Al-Si-N films was investigated in detail. It was found that the Al-Si-N films are crystalline, highly elastic and optically transparent, and exhibit (i) the columnar microstructure and low resistance to cracking when sputtered at low Ebi, (ii) the non-columnar, voids free microstructure and the enhanced resistance to cracking when sputtered at high Ebi. Recently, the flexible nanocomposite films which exhibit an enhanced resistance to cracking exhibit simultaneously all necessary parameters, i.e. high ratio H/E* ≥ 0.1, high elastic recovery We ≥ 60%, dense, voids-free microstructure and compressive macro-stress σ; here H is the hardness, E* is the effective Young's modulus. These properties can be achieved by optimization of the deposition parameters used in sputtering. Our experiment clearly shows that all necessary parameters can be controlled by the one deposition parameter, i.e. by the energy Ebi delivered to the film during its growth. This is the fundamental finding of high scientific value which opens new possibilities in the formation of advanced thin films and coatings. The energy is a key parameter in the formation of films with prescribed properties in a reproducible way.

Authors : Bilal Istanbullu, Mahmut Kus
Affiliations : Bilal Istanbullu; Selcuk University, Advanced Technology Research and Application Center, Konya/TURKEY Selcuk University, Department of Nanotechnology and Advanced Materials, Konya/TURKEY Mahmut Kus; Selcuk University, Advanced Technology Research and Application Center, Konya/TURKEY Selcuk University, Departmant of Chemical Engineering, Konya/TURKEY

Resume : Organic Field Effect Transistors (OFETs) have been gaining considerable interest by researchers due to their role in electronic devices. Because of its’ huge effect on device performance, device structure of OFETs is important as much as semiconductor and dielectric layers. There are many OFETs with different geometries such as linear, interdigitated, etc. improved to produce high performance thin film transistors (TFTs). Here in, we go over a comparative study on fabricating OFETs with different geometries where the source and drain electrodes are patterned by using photolithography method. PCBM as semiconductor and poly(1-vinyl-1,2,4-triazole) (PVT) as dielectric layer were used to fabricate OFETs. We investigated the effect of different geometries on TFT performance.

Authors : Dhafer Abdelkader, Ferid Chaffar Akkari, Naoufel khemiri, Frédéric Antoni, Bruno Gallas, Mounir Kanzari
Affiliations : 1.Laboratoire de Photovoltaïque et Matériaux Semi-conducteurs-ENIT-Université Tunis ElManar,BP37,Lebelvédère 1002 Tunis-Tunisia 2. ICube-Laboratoire des sciences de l’Ingénieur, de l’Informatique et de l’Imagerie, Université de Strasbourg-CNRS, 23, rue du Loess, 67037 Strasbourg Cedex, France 3. Institut des NanoSciences de Paris-CNRS-Université Pierre et Marie Curie, 140 rue de Lourmel, 75015 Paris, France

Resume : SnSb4S7, Sn2Sb6S11, SnSb2S4, Sn4Sb6S13, Sn2Sb2S5 and Sn3Sb2S6 thin films were prepared by thermal evaporation using the glancing angle deposition technique (GLAD). The GLAD is implemented to produce inclined columnar structures. The incident angle between the particle flux and the normal to the substrate is fixed at 80°. The XRD and Raman characterizations revealed amorphous films due to the columnar structure of the films shown by the SEM and AFM characterizations. The surface roughness increases with the SnS addition. A strong change of the surface morphology of the films was observed and it depends to the composition. The FTIR spectra exhibit a noticeable changement comparing with the ones of as deposited samples.Optical properties were extracted from transmittance T and reflectance R spectra. SnxSbySz thin films exhibit high absorption coefficients (104 - 2×105 cm-1) in the visible range and the higher values were obtained for Sn3Sb2S6. The direct band gap (Eg dir) and indirect band gap (Eg ind) were in the range 2.11 – 1.67 eV and 1.87 – 1.42 eV, respectively. The refractive indices are calculated from optical transmittance spectra of the films for wavelengths from 300 to 1800 nm. The Sn3Sb2S6 sample exhibits the lower refractive index. The complex dielectric constant (ε'', ε') were calculated and then the cole-cole plots show a dielecric relaxation. The dielectric tangent loss δ and the optical conductivity (σ opt) were derived. The Bruggeman effective medium approximation EMA was used to calculate the packing density of different compositions, and Sn2Sb2S5 sample has the highest value of packing density.

Authors : Paramita Patra1*, S. A. Khan2, D. Kabiraj2, Manju Bala2, D. K. Avasthi3, S. K. Srivastava1
Affiliations : 1 Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721302, India 2 Inter-University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110 067, India 3 Amity University, Noida, Uttar Pradesh 201313, India *Email:

Resume : Irradiation of thin films with energetic ions often leads to atomic displacements due to the ion-matter interaction, resulting in order to produce novel materials, phase transformation and interface mixing. In the case of swift heavy ions (SHIs), the occurrence of thermal spikes via electron-phonon coupling (EPC) mediated transfer of electronic energy to lattice [1,2] has been identified as the primary cause of all observed SHI-matter interaction related phenomena. In order to estimate or predict the effect of SHI irradiation quantitatively, the EPC factor has so far been taken to be constant equal to the electron density of states (eDOS) at Fermi energy according to the free-electron theory of metals. However, in metals, the electrons are under a highly non-equilibrium process and the calculation of EPC factor requires exact eDOS, which can be computed from density functional theory (DFT) [3]. Based on the above concept, we calculated composition-dependent EPC strength for a series of complete solid soluble Pd1-xNix alloys by computing their eDOSs using full-potential linearized augmented plane wave method of DFT and indeed found an x-dependence of EPC strength for the alloy system. In order to see its effect on SHI-matter interaction, we prepared these alloys on Si substrates, irradiated these with 100 MeV Au ions at 1x10^14 ions/cm^2, and monitored the diffusions of Pd and Ni independently in Si for each case. Although the Rutherford backscattering spectra do not show any intermixing possibly due to the poor spatial resolution of the technique, the depth profiles using X-ray photoelectron spectroscopy show a considerable mixing of Pd and Ni in Pd/Si and Ni/Si systems, respectively, right after the SHI irradiation, an observation not reported earlier for these systems. Further, for an intermediate composition Pd1-xNix, the mixing efficiencies of Pd and Ni both in Si is found to be an order of magnitude less than those of pure elements. This is in complete agreement with the notion that the EPC factor must be calculated using eDOS, rather than taking as a constant and thus supports the thermal spike model of SHI-matter interaction. References: 1. Z.G. Wang, C. Dufour, E. Paumier and M. Toulemomde, J. Phys: Condensed Matter, 6 (1994) 6733 2. S.K. Srivastava, D.K. Avasthi, W. Assmann, Z. G. Wang, H. Kucal, E. Jacquet, H. D. Carstanjen and M. Toulemonde, Phys. Rev. B 71 (2005) 193405. 3. Z. Lin, L.V. Zhigilei, and V. Celli, Phys. Rev. B 77 (2008) 075133.

Authors : V. Satulu1, B. Mitu1, S.I. Voicu2, L. Kravets3, G. Dinescu1
Affiliations : 1 National Institute for Lasers, Plasma and Radiation Physics, PO Box MG-36, 077125 Magurele Bucharest, Romania 2 Politechnical University of Bucharest, Faculty of Applied Chemistry and Material Science, Gh. Polizu Str. 1-7, S1, 011061 Bucureşti, Romania 3 Joint Institute for Nuclear Research, Flerov Laboratory of Nuclear Reactions, Joliot-Curie Str. 6, 141980 Dubna, Russia

Resume : Membrane separation is a promising technology for wastewater treatment as well as for particles, microorganisms and organic/inorganic pollutants removal from aqueous solutions. The polymeric porous membranes used in membrane separation technology are highly affectted by the chemicals to be filtered, limiting their prolonged use. In this context there is an important interest for obtaining of new membrane separation systems with enhanced chemical resistance. In this work, we describe the synthesis and characterization of thin films composite (TFC) membranes based on thin films deposited on polymeric porous supports with improved filtration properties. Polyethylene terephthalate track etched membranes (PET-TM) were used as porous substrates, while chemically-resistant polytetrafluoroethylene (PTFE)-like thin films were deposited as protective layer by RF magnetron sputtering. The influence of substrate pores size on the morphological characteristics of the TFC membranes surface was investigated by means of Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) techniques. The chemical composition of initial and thin films composite membranes with various pores diameters was revealed through Fourier Transform Infrared Spectroscopy (FTIR) and X-ray Photoelectron Spectroscopy (XPS) investigations. The thin film composite membranes has been tested as regarding the retention of Albumine Serum Bovine (ASB) and filtration of solvents. This work has been financed by the Romanian Ministry of Research and Innovation in the frame of Nucleus programme-contract 4N/2016.

Authors : Adriana BALAN (1), Alice O. MATEESCU (2), Catalin CEAUS (1), Gheorghe MATEESCU (2), Ioan STAMATIN (1), Sanda VOINEA (1), Cornel SAMOILA (3), Dan CRISTEA (3)
Affiliations : (1) University of Bucharest, Faculty of Physics, 3 Nano-SAE Research Centre, 405 Atomistilor Str., 077125 Magurele, Romania (2) ”Horia Hulubei” National Institute of Physics and Nuclear Engineering, 30 Reactorului Str., 077125 Magurele, Romania (3) Transilvania University of Brasov, Materials Science Department, 29 Eroilor Blvd.,500036, Brasov, Romania

Resume : Tungsten Disulfide (WS2) is a low friction dry lubricant coating that improves performance and service life by reducing friction, improving mold release and solving problems related to wear, seizing, galling and fretting. A variety of deposition technics for transition-metal dichalcogenides thin films has been employed, such as sputtering, ion beam sputtering and pulsed laser beam deposition. In this paper, WS2 nanostructured thin films are obtained by Low Pressure Cold Spray deposition, a still untapped technique for such materials. The material desired design is a parallel position of the van der Waals-planes to the substrate surface, the formation of thermally stable and hard phases WS2 films, resulting in superior mechanical and tribological properties. The microstructure of these coatings was thoroughly analyzed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Corrosion resistance of the coated steel was examined in 0.1M aqueous NaCl solution by potentiodynamic polarization and electrochemical impedance spectroscopy, while tribological characteristics were determined by scratch, hardness test method and Pin-on-disk Tribometer measurements. The influence of the WS2 films properties, such as number of layers, the surface roughness parameters and morphology on corrosion resistance and tribological characteristics of stainless steel is addressed.

Authors : M.A.Vasylyev1, B.N. Mordyuk1, S.I.Sidorenko2, S.M.Voloshko2, A.P.Burmak2
Affiliations : 1Kurdyumov Institute for Metal Physics of the NAS of Ukraine, Ukraine; 2Metal Physics Department, Igor Sikorsky Kyiv Polytechnic Institute, Ukraine.

Resume : Ultrasonic impact treatment (UIT) of stainless steel 321 was carried out at room temperature in the air and argon environments and at cryogenic (liquid nitrogen) temperature in quasi-isostatic conditions with application of the same mechanical energy applied to specimens. The microstructural evolution in the surface layers of the deformed specimens was studied by XRD, SEM and TEM analyses. The volume fractions of the deformation-induced alpha- and epsilon- martensites were estimated using XRD approach and magnetic measurements of saturation magnetization. Compared to room temperature UIT (RT-UIT), liquid nitrogen UIT (LN-UIT) generates a higher density of deformation twins and stacking faults. In addition, a higher volume fraction of alpha-martensite (~53%) and retained epsilon-martensite (~3,5%) were observed after LN-UIT in deeper surface layers (~200 μm). This is due to the increase in the density of potential embryos for martensite nucleation by deformation at cryogenic temperature. After LN-UIT, a nanoscale grain structure of heterogeneous nature (martensite and austenite phases) occurs simultaneously with the areas filled with networks of deformation twins and stacking faults. Both types of microstructure contribute to material strength and result in higher hardness of the LN-UIT processed specimens (~5–6.55GPa) compared to that of the RT-UIT processed ones (~3GPa). To achieve enhanced corrosion resistance in saline solution the single phase nanostructure is required.

Authors : Maria Covei, Alexandru Enesca, Cristina Bogatu, Dana Perniu, Anca Duta
Affiliations : R&D Centre: Renewable Energy Systems and Recycling, Translvania University of Brasov, Romania

Resume : The use of protective coatings for photovoltaic glazing represents a hot topic at EU level, as an alternative method to increase electrical output. One challenge is to simultaneously meet a set of optical properties in the full solar spectral range: high transmittance (T%) - low reflectance (R%) in UV-Vis and low T% - high R% in IR (IR-shielding); additional self-cleaning features represent a functional asset. Following the optical and the self-cleaning pre-requisites, a novel, sol-gel composite using WO3 and reduced graphene oxide (r-GO) was obtained. Tungsten precursors (WCl6, WOCl4 or H2WO4) along with r-GO (0..5% wt.) were dispersed in water-ethanol mixtures (ratios of 1:0, 0:1 and 1:1). Acetylacetone and SDS at concentrations higher and lower than the critical micelle concentration were used to control particle nucleation and growth. The sols were aged for 48 h, dried and annealed at 550oC. The synthesis parameters were correlated with crystallinity, morphology, surface energy and optical properties of the powders. Stable dispersions were prepared using the powders with high TUV-Vis - low TIR and chitosan, to be sprayed on solar glass. The results show that homogeneous, transparent thin films can be obtained using dispersions at optimized pH and concentration; the number of spraying sequences and the deposition temperature (40…60oC) are key parameters in controlling the optical and self-cleaning properties (the latest being tested in 20 ppm phenol removal).

Authors : Asghar Heydari Astaraee, Reza Miresmaeili, Mahmood Aliofkhazraei, Sara Bagherifard, Mario Guagliano
Affiliations : Department of Materials Engineering, Tarbiat Modares University, P.O. Box: 14115-143, Tehran, Iran; Department of Materials Engineering, Tarbiat Modares University, P.O. Box: 14115-143, Tehran, Iran; Department of Materials Engineering, Tarbiat Modares University, P.O. Box: 14115-143, Tehran, Iran; Department of Mechanical Engineering, Politecnico di Milano, 20156 Milan, Italy; Department of Mechanical Engineering, Politecnico di Milano, 20156 Milan, Italy

Resume : Gradient microstructures on surface of metals by severe shot peening (SSP) is relatively a new research topic in the field of severe plastic deformation processing. The treated surface is known to show three distinct features: a spectrum of grain size from nanometer to sub-micron to micron regime, work-hardened surface layer, and a compressive residual stress profile near the surface. The current study is defined to investigate the effects of SSP preprocessing on the anodization behavior of Aluminum. Gradient microstructures were obtained on AA1050 Al substrate using SSP with different coverage levels. SSP was performed with ceramic media to prevent contamination of the treated surface. Then the treated surface was anodized at constant voltages in a sulfuric acid solution. The Current-time responses were recorded to reveal the surface reactivity. It was found that the refined microstructure of Al substrate enhances the growth rate of Anodic oxide. A variable growth rate is detected within the treated layer. The growth kinetics of anodic oxide is discussed in terms of underlying oxide formation mechanisms and extent of surface grain refinement.

Authors : Doohun Kim
Affiliations : Korea Electrotechnology Research Institute

Resume : V203 thin films were prepared by the reduction of sol-gel derived vanadium oxide films. The films were examination by x-ray diffraction, SEM, TEM, and atomic force microscopy. The films annealed under controlled oxygen atmospheres show a typical metal-insulator transitions characteristic. We applied the V2O3 thin film in the 2G high temperature superconductivity coil as a interlayer for current bypassing.

Authors : Jun-Gyu Choi, Won-June Lee, Myung-Han Yoon*
Affiliations : School of Materials Science and Engineering, Gwangju Institute of Science and Technology, South Korea

Resume : The metal oxide semiconductor is one of the promising materials for large-scaled flexible electronics due to their high optical transparency, mechanical flexibility and electrical properties. Moreover, the carrier transporting property of the metal oxide semiconductors is not affected by their phase structure due to their non-directional orbital structures, so amorphous metal oxide semiconductors can have relatively high mobility and on-off current ratio without crystallizing process. However, it has been recently reported that the bias stability could be improved by enhanced crystallized structure. Nevertheless, high processing temperature above 350°C for high crystallinity remain the obstacle in terms of flexible application and manufacturing process. In this work, the solution-processed indium oxide semiconductor could be crystallized at 200? by the combustive reaction of the ammonium-based metal precursor under the deep-ultraviolet(DUV) radiation. It was observed that the intensive exothermic reaction was carried out in the ammonium-based metal precursor solution around 200°C, resulting that the crystallization was reinforced at low processing temperature. Moreover, the additional optical energy from DUV radiation could reduce the ignition temperature of additive, improve the crystallinity, and enhance the electrical mobility. We can expect that these synergistic reactions can enhance the reliability of conventional metal oxide-based devices at low processing temperature.

Authors : Irfan Haider Abidi, Abhishek Tyagi, Zhengtang Luo
Affiliations : Department of Chemical and Biomolecular Engineering, Hong Kong University of Science and Technology, Clear Water Bay, Kowloon, Hong Kong

Resume : We reported a unique strategy to constrain the nucleation centers for multilayer graphene (MLG) and later single-crystal graphene domains through gettering the carbon source on backside of the flat Cu foil, during chemical vapor deposition (CVD). Hitherto, for a flat Cu foil, merely top-surface-based growth mechanism has been emphasized during CVD growth, while overlooking backside graphene. However, our systematic experimental findings indicated the strong correlation between backside graphene and MLG growth on the top surface, which governs by the carbon diffusion through the bulk Cu. This understanding steers us to devise a strategy of mitigating carbon diffusion to the top surface by using a “getter” substrate such as nickel for carbon at backside of the Cu foil. Later, depth profiling of the nickel substrate, along with Density Functional Theory (DFT) calculation, verifies the gettering role of nickel support. Implementing, backside carbon gettering (BCG) approach to single-crystal graphene growth resulted in lowering of the nucleation density by two orders of magnitude, enabling growth of single-crystal domains of ⁓ 6 mm lateral size on untreated Cu foil. Finally, we demonstrate the growth of large area polycrystalline SLG, free of unwanted MLG domains, with significantly improved field-effect mobility of ~ 6800 cm2V-1s-1 and 97.7% transmittance, offering potential for high-performance optoelectronic device applications. Our approach provides an unusual methodology for control in chemical vapor deposition of 2D materials.

Authors : R. Pietruszka1, B. S. Witkowski1, S. Zimowski2, T. Stapinski3, M. Godlewski1,4
Affiliations : 1Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw, Poland 2AGH University of Science and Technology, Faculty of Mechanical Engineering and Robotics, Mickiewicza Av. 30, 30-059 Krakow, Poland 3AGH University of Science and Technology, Mickiewicza Av. 30, 30-059 Krakow, Poland 4Department of Mathematics and Natural Sciences College of Science, Cardinal Stefan Wyszynski University, Warsaw, Poland

Resume : Atomic layer deposition (ALD) method is commonly used to deposit oxide, nitride and sulfur layers for selected industrial applications. Currently, a big potential of the ALD method in photovoltaic (PV) applications is demonstrated for aluminum oxide (Al2O3), zinc oxide (ZnO) and aluminum doped zinc oxide (AZO) thin films. ALD-grown ZnO and AZO layers are cheap alternatives to expensive ITO (Indium Tin Oxide). Moreover, passivated layers based on Al2O3 (ALD-grown) are already applied in the production of crystalline silicon PV structures. The possibility of mass production by the ALD technology raises the question, how mechanically strong, stable and hard are ALD-grown oxide layers? In this work, we study oxide layers grown by the ALD method on glass substrates. Tribology, hardness, friction coefficient and Young modulus are investigated. The results indicate a good adhesion of ZnO films to substrates. Even with a load of 10 N these films maintain a resistance to wear of up to 500 cycles during sliding against alumina ball with 6 mm of diameter. The friction coefficient of ZnO film is 0.1, and retains its value during the test. The tribological properties of the ALD-grown oxide films are compared with those reported for bulk substrates and films deposited by a sputtering method. This work was partially supported by the National Science Center (Decision Nos. DEC-2012/06/A/ST7/00398 and DEC-2013/11/B/ST7/01385), and AGH, AGH

Authors : David Roilo, Cecilia Ada Maestri, Paolo Bettotti, Marina Scarpa, Riccardo Checchetto
Affiliations : David Roilo; Cecilia Ada Maestri; Paolo Bettotti; Marina Scarpa; Riccardo Checchetto Department of Physics, University of Trento, via Sommarive 14, I-38123 Povo, TN, Italy.

Resume : Nanocellulose and nanocellulose composites have gained increasing attention in recent years for applications in the packaging technology, given important properties as biodegradability, high optical transparency and gas barrier. [H. Fukuzumi et al., Biomacromolecules 2013, 14, 1705] Cellulose nanofibers films having thickness in the few micrometer range were deposited by solution casting [P. Bettotti et al., Adv. Mater. Interfaces 2015, 1500415] on a polylactic acid substrate, which is a bio-derived and biodegradable material representing a promising alternative to petrochemical-based polymers for packaging. The transport kinetics of light gases in the bilayer membranes was studied as a function of the coating thickness by time resolved mass spectrometry [R. Checchetto et al., Meas Sci Technol 1995, 6, 1605] using gases with different size and condensation properties, to evaluate the diffusivity and solubility of the test gases in the TOCN coatings and their temperature dependence. With this information, it is possible to shed light on the transport mechanism of gases in the nanocellulose coatings and explain the reason of the excellent gas barrier properties.

Authors : Dooyong Lee1,3, Hyegyeong Kim1, Sehwan Song1, Ji Woong Kim1, Ik Jae Lee2, Yooseok Kim3, Hyung-Joong Yun3, Jouhahn Lee3, Sang-Don Bu4, Sungkyun Park1,*
Affiliations : 1 Department of Physics, Pusan National University, Busan 46241, Korea ;2 Energy & Environmental Materials Team, Pohang Accelerator Laboratory, Pohang 37673, Korea ;3 Advanced Nano Surface Research Group, Korea Basic Science Institute, Daejeon 34133, Korea ;4 Department of Physics, Chonbuk National University, Jeonju 54896, Korea

Resume : Vanadium dioxide (VO2) has been extensively studied not only its fundamental interests in the origin of a phase transition but also its potential applications in many modern devices. Recently, many researchers have studied to control the phase transition temperature (TC) and ?TC and/or the degree of resistivity changes (??) during the transition by various methods such as doping, chemical substitution, ion implantation, varying growth environments, etc. Among them, light elements doping can be useful in many senses. In particular, the surface of VO2 provides catalytic site for hydrogen dissociation, hydrogen can be easily incorporated and dissociated in the VO2. In this presentation, we investigated the effect of hydrogen in metal-insulator-transition (MIT) of the as-grown and post annealed VO2 films [1]. The epitaxial film was grown on Al2O3(0001) using RF sputtering at 600 oC and annealed under hydrogen environment (~0.3 mbar) at various temperatures (RT ~ 300 oC). X-ray diffraction (XRD) showed both as-grown and annealed films have a (020) orientation. However, the annealed film at 300 oC under hydrogen gas exhibited lower 2? value due to hydrogen intercalation. The electrical measurements showed that no MIT was observed in the annealed film. On the contrary, as-grown film observed the transition at 55.20 oC (heating) and 49.26 oC (cooling). This observation suggested the existence of structural change from monoclinic to rutile in the annealed film. The in-situ chemical state variation was also monitored using ambient pressure X-ray photoelectron spectrometer during hydrogen annealing. As a results, the V4 state was changed into the various valence states during hydrogen annealing. In addition, an increase in octahedral symmetry after hydrogen annealing was observed by X-ray absorption spectroscopy measurement. [1] D. Lee et al., Appl. Surf. Sci. 396 (2017) 36-40. This research is supported in part by NRF Korea (NRF-2015R1D1A1A01058672), Korea Atomic Energy Research Institute and Korea Basic Science Institute (E36800). Also, J. W. Kim is supported by Global PhD Fellowship Program through the NRF Korea funded by the Ministry of Education (2015H1A2A1034200). *E-mail:

Authors : I-Wen Wang 1, Jeng-Ting Li 1, Jen-Sue Chen 1, and Jiann-Shing Jeng 2
Affiliations : 1 Department of Materials Science and Engineering, National Cheng Kung University, Tainan 70101, Taiwan; 2 Department of Materials Science, National Tainan University, Tainan 70005, Taiwan

Resume : In this work, ultra-thin ZTO films (~5nm) prepared by a solution route have been applied as the active semiconductor layer in a thin film transistor (TFT). We choose zinc-tin oxide (ZTO) instead of indium-gallium-zinc oxide (IGZO) to avoid expensive In and Ga elements.The purpose of using solution process is owing to its advantages of low cost and feasibility for large area deposition. Due to the large bandgap of Zn-based oxide semiconductors (>3.3eV), the photoresponse is limited in the UV region. After incorporating a dye which can absorb longer wavelength, the photo-excited electrons in the dye transferred to ZTO, enhancing the photoresponse of our ZTO TFT in the visible light region. With light illumination of 532nm wavelength, the photosensitivity of dye-sensitized ZTO TFT is >10^5 and the photoresponsivity is improved for eight times, reaching 866A/W. Therefore the dye-sensitized ZTO TFT has broad spectral photodetectivity and is widely applicable.

Authors : M. Duris1.2., D. Deubel.1, L. Bodiou.2, C. Vaudry.1, J-C Keromnes.1 and J. Charrier.2,
Affiliations : 1.KERDRY, 5 Rue Louis de Broglie, 22300 Lannion, France; 2.CNRS UMR 6082 Foton, ENSSAT CS 80518, 22305 Lannion, France

Resume : The development of new products and the need to enhance material functionalities requires the optimization of the multilayered structure to respond to the increasing of request in mid-infrared (Mid-IR) applications such dichroïc or bandpass filters. The development of Mid-IR applications requires the implementation of new discrete optical components. These new products with enhanced functionalities can only be achieved by optimization of the coating. To manufacture theses optical multilayered structures, Germanium and Zinc Sulfide thin layers can be good candidates thanks to the sufficiently large refractive index contrast (Δn~1.9) and high optical transmission of individual materials in wavelength range of interest. Multilayered structures were manufactured by e-beam evaporation process. The refractive indices of germanium and zinc sulfide layers are investigated as a function of deposition parameters (rate, pressure, substrate temperature) from reflectance and transmittance spectra measured by FTIR spectroscopy. The optical design based on Ge and ZnS films is presented by taking into account the thickness and refractive index deviations of the deposited layers. Successful result of antireflective coatings on silicon or germanium substrates is then demonstrated in the Mid-IR range. A high transmittance coating was fabricated on a silicon substrate; the result of a 4-layered Ge-ZnS structure covers 3500 - 4500 nm spectral band giving bandwidth ~ 1000 nm and a transmittance of ~ 70%.

Authors : A.V. Vasin*, A.V. Rusavsky*, I.P. Neshpor**, T.V. Mosina**, D.V. Vedel**, O.N. Grigoriev**, A.N. Nazarov*
Affiliations : *Lashkaryov Institute of Semiconductor Physics NAS of Ukraine, Kyiv, Ukraine; **Frantsevich Institute of Materials Science Problems NAS of Ukraine, Kyiv, Ukraine

Resume : Effect of amorphous SiOC(:Er) coatings on oxidation behavior of ZrB2-SiC composite ceramics was studied. Samples of ZrB2–15%SiC composite were obtained by hot pressing method without protective atmosphere of ZrB2+15%SiC powder at 1850оС and 48 MPa. Amorphous SiOC(:Er) thin films were deposited on ZrB2-SiC specimens at temperature of 200 oC by reactive RF-magnetron sputtering of crystalline SiC target in argon/oxygen flow. Surprisingly, ZrB2–SiC specimen revealed 100 % increase of bending strength after coating with 1 micron SiOC layer. Coated ZrB2-SiC samples were exposed to high-temperature oxidation at 1400 oC for an hour at atmospheric pressure. Structure and phase analysis of a near surface layer were analyzed by examination of metallographic cross-sections by optical microscopy, X-ray diffraction, EPMA and photoelectron spectroscopy. It was demonstrated that SiOC coating noticeably enhance oxidation resistance of the surface. Further development of oxidation resistance was observed in Er-incorporated SiOC coating. Development of surface stability by SiOC(:Er) coating is attributed to high density and high homogeneity of the coatings deposited at low temperature using crystalline SiC target and increased viscosity as well as melting point caused by Er incorporation.

Authors : Catalin Vitelaru, Iulian Pana, Adrian Kiss, Nicolae Catalin Zoita
Affiliations : National Institute for Optoelectronics, 409 Atomistilor St., 077125 Magurele, Romania ; Faculty of Physics, University of Bucharest, 405 Atomistilor St., Magurele 077125, Romania

Resume : Copper-oxide is a material adaptable for many applications, with different properties depending on the oxidation state and the production technique. The optical band gap tunability of CuOx obtained by reactive sputtering process of Cu target under DC bias in Ar/O2 gas mixture was investigated. The hysteresis behavior of reactive process was evaluated under different control modes, keeping constant either the pressure, total gas flow or pumping speed. Optical emission spectroscopy, partial and total pressure measurements and discharge electrical parameters were used to describe the reactive process. By adjusting the gas flows, to account for the pumping speed difference for Ar and O2, it was possible to separately evaluate the oxygen gas losses due to the reactive processes inside the plasma chamber. Thin films of CuOx were deposited and characterized, for a selected number of critical points on the process window. The transition from Cu rich layer to CuO, going through different types of Cu2O layer was assessed by XRD analysis. The optical band gap values, determined by using the absorption spectra fitting method according to Tauc model, indicated a variation from 1.09 eV to 1.85 eV by decreasing the O2 flow ratio from 56 to 19% of total flow. Moreover, a good concordance between the variations of process parameters and thin film properties was obtained. We acknowledge the support of the Romanian Research and Innovation Ministry, projects PN, PN

Authors : L.R. Constantin, A.C. Parau, M. Dinu, M. Balaceanu, A. Vladescu, M. Braic
Affiliations : National Institute for Optoelectronics, 409 Atomistilor St., Magurele-Bucharest, 077125 Romania; Phone/fax: +4021-457 57 59

Resume : Ternary transition metal carbonitride coatings containing abundant elements, such as TiCN, CrCN and ZrCN are known as excellent protective coatings against wear, erosion and corrosion [1,2 ]. This work aims to assess the influence of Cr and Si addition on the tribological characteristics of ZrCN based coating. The ZrCN and ZrCrSiCN coatings (~ 3.7 µm thick) were deposited on C 45 steel substrates by the cathodic arc method, in a mixture of C2H2 and N2. The coatings were investigated in terms of elemental composition, microstructure, mechanical properties and tribological performance, and compared to uncoated C 45 steel discs. The addition of Cr and Si to ZrCN coating determined the decrease of the grain size, indicating an amorphisation process, specific for Si addition. The observed hardness enhancement and improved friction and wear performance in dry test conditions was ascribed to the formation of an amorphous silicon carbonitride phase at grain boundaries, as well to the superior friction characteristics of Cr compounds. The obtained results recommend ZrCrSiCN coatings to be used in tribological demanding industrial applications. We acknowledge the support of the Romanian Research and Innovation Ministry, projects PN and PN-III-P2-2.1-PED-2016-1580. 1. M.Braic, A.Vladescu, M.A.Morris et al., Appl. Surf. Sci., doi: 10.1016/j.apsusc.2016.12.160 2. C.I.Pruncu, M.Braic, K.D.Dearn et al., Arabian Journal of Chemistry, doi:10.1016/j.arabjc.2016.09.009

Authors : M.Yu. Verbytska, Ye.О. Kholina, P.V. Makushko, T.I. Verbytska, S.I. Sidorenko, Yu.M. Makogon
Affiliations : National Technical University of Ukraine «Igor Sikorsky Kyiv Polytechnic Institute», 03056, Prospect Peremogy 37, Kyiv, Ukraine

Resume : Heat treatment of Fe/Pt multilayers has recently attracted attention as a possible way for the synthesis of hard magnetic L10 FePt thin films for high-density magnetic recording devices. The purpose was to investigate the effect of annealing atmosphere and thickness of layers on L10 phase formation. Pt(4.2 nm)/Fe(3.2 nm)]4 and [Pt(2.1 nm)/Fe(1.6 nm)]8 films were deposited by magnetron sputtering on SiO2(100 nm)/Si(001) substrate at RT. Heat treatment of the samples was carried out in vacuum and in N2(RTA) in the range of 500 - 900ºC for 30 s. The films were investigated by XRD, SQUID and AFM. The as-deposited [Pt/Fe]4 sample exhibits satellite reflections around the solid-solution peak due to layered structure. The increase in number of layers at reducing of layer thickness promotes in activation of diffusion processes on the interfaces and leads to shift satellite and solid-solution reflections in side of smaller and larger angles, accordingly. A1 → L10-FePt phase transformation in annealed in vacuum films takes place at 700°C. RTA due to tensile in-plane strain promotes to L10-FePt phase formation at 600°C and the growth of (001) - oriented grains in both films. The greater amount of grains oriented in [001] directions perpendicular to substrate is formed in [Pt/Fe]4 films annealed as in vacuum as in N2 atmosphere. Additional number of interfaces prevents the grain growth. In films after RTA the magnetic properties are improved and film's roughness is decreased.

Authors : Maryam Saeed, Ian Kinloch, Brian Debry
Affiliations : University of Manchester

Resume : Chemical vapour deposition (CVD) of graphene on liquid substrates is a potential production route for large area, single domain monolayer graphene due to the uniformity of a liquid surface. The catalytic potential of transition metals for CVD graphene is well established. Liquid copper (Cu) substrates have shown excellent results for growing homogenous and uniform graphene films grown on low melting point liquid metals and alloys, namely liquid tin (Sn) and five different compositions of Cu:Sn alloys. All films were grown at temperatures significantly greater than the alloy melting point under conditions of flowing Ar and H2 with CH4 as the hydrocarbon feedstock. The influence of temperature, gas composition and flow rate on graphene growth and quality was studied. It was found that higher temperatures lead to better methane cracking on the molten Sn surface, and that the graphene grain size increases with increasing residence time leading to lower defects density in resulting film. The alloy composition was found to strongly influence the number of graphene layers with Cu20%:Sn80% gave bilayer graphene. Finally, we demonstrate a novel direct graphene transfer method from liquid substrate onto a range of target substrates such as SiO2 and polyimide (PI).

Authors : D. Kourtidou, D. Chaliampalias, D. Karfaridis, C. Vogiatzis, E. Pavlidou, P. Patsalas, S.Skolianos, K. Chrissafis, G. Vourlias
Affiliations : Aristotle University of Thessaloniki

Resume : Oxidation is a common problem in steel constructions, with economic and environmental consequences. However its good mechanical properties, steel oxidizes quickly and easily, especially in elevated temperature environments which in turn lower its structural integrity. High temperature, wear and oxidation durability can be achieved by developing a coating layer of proper materials with improved properties. Nickel and Aluminum are ideal materials for such applications and have been claimed to possess high-temperature mechanical strength and oxidation resistance. In this work such coatings were prepared by a combination of two processes which are simple, economic and environmental friendly comparing with the already used techniques. An initial Ni layer was electrochemically deposited on steel followed by Al deposition via pack cementation thermochemical process. The structure and phase identification was performed using X-ray diffraction and X-ray photoelectron spectroscopy, while the morphology and elemental analysis was examined by Scanning electron microscopy. The deposited coatings were found to contain Ni-Al phases, mainly Al3Ni2 and AlNi3. Moreover, Ni-Fe phases were also formed at the substrate/coating interface, due to the diffusion of Ni layer in the substrate during thermal treatment at the aluminization step. Thermogravimetric and electrochemical corrosion measurements revealed a significant increase of the samples resistance comparing to the uncoated steel.

Authors : S.I. Sidorenko, G.G. Lobachоva, Ie.V. Ivashchenko, N.A. Shapovalova, K.V. Melashenko
Affiliations : Metal Physics Department, Igor Sikorsky Kyiv Polytechnic Institute, Ukraine.

Resume : The one of the main directions in modern material science is creating new hard and wear resistant coatings with increased physicochemical and operational properties. A promising method of creating, which operated in extreme conditions, is electric-spark alloying. In this method by means of concentrated flows of electric energy, surface layer chemical composition, structure-phase state and properties is being modified. In this work investigated influence of combined treatment with previous electric-spark surface alloying with copper and chrome in different sequences and subsequent shock treatment on structure, microhardness, and wear resistance of low-carbon steel surface layers. Discovered, that with changing the sequence of alloying with chrome and copper lead to surface micro hardness changes. The highest microhardness have coatings with chrome top layer, due to the formation of oxides and carbides during its interaction with oxygen and carbon in steel base in conditions of high-temperature, ultra-high heating and cooling rates. Proved, that the shock treatment after alloying increasing microhardness and wear resistance. The highest grade of deformation have samples with copper top layer. Offered model of structure-phase transformations of steel surface layer in electric-spark alloying process.

Authors : Nicolae-Catalin ZOITA, Adrian Emil KISS, Mihaela DINU, Catalin VITELARU, Viorel BRAIC
Affiliations : National Institute of Research and Development for Optoelectronics (INOE 2000)

Resume : Titanium carbide (TiC) is a well-known refractory material due to its valuable physical and chemical properties, which are very attractive for the scientific and technological communities. TiC presents excellent electrical and thermal conductivity, high hardness, high chemical stability and good corrosion resistance. For applications like high power electronics, which require low electrical resistivity films, ohmic contacts made of single-crystalline TiC layers proved valued solutions. Up to now, epitaxial TiC films have been fabricated by both CVD and PVD techniques, the co-evaporation of metallic Ti and C60 as well as the magnetron sputtering proved valuable technics for epitaxial growth at low substrate temperature. In a previous work, our team obtained by reactive sputtering of Ti target in CH4 atmosphere TiC epitaxial layers with electrical resistivity as low as 160 μΩ cm. In order to improve the crystalline quality and the electrical conductivity of epitaxially grown TiC films, in this work a hybrid magnetron co-sputtering technique was considered, where the Ti target was sputtered in DC mode while the C target in HiPIMS mode. TiC samples grown on MgO(100) at different substrate temperatures are compared in terms of morphological, structural and electrical properties with samples grown by reactive sputtering technique. We acknowledge the support of the Romanian Research and Innovation Ministry, projects PN, PN

Authors : Edson M. Santos, D. Faurie
Affiliations : Universidade do Estado da Bahia- UNEB; LSPM-CNRS, Université Paris XIII, Sorbonne Paris Cité

Resume : The purpose of the present article is to make a model using analytical equations, based on elasticity theory of continuous media for small deformations, with the aim of completely characterizing the material in their mechanical properties as well as the principal stress-strain of thin films. Therefore, the constitutive relation between strain and stress will be considered orthotropic, obeying the generalized Hooke's law. A new equation for the stress of the film-substrate system is proposed based on Newton's laws and energy conservation. As an application, we use the technique and data developed by Faurie et al (2005) in fiber-textured gold film deposited onto Kapton substrate by combining synchrotron X-Ray diffraction in situ tensile testing. It is firstly required a texture analysis with the purpose of determining the possible (psi) angles for each crystallographic directions that can be used in the model equations. With the data, it is possible to make graphics, for example, strain X F, for every force applied to the sample. We obtain this procedure from their mechanical properties and the principal stress-strain of the anisotropic gold thin film. Our results are compared with the results of Faurie et al (2005).

Authors : Jung Hye Lee1, Hak-Jong Choi2, Heon Lee2, Yeon Sik Jung1
Affiliations : 1Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology (KAIST), Daejeon 34141, Korea; 2Department of Materials Science and Engineering, Korea University, Seoul, 02841, Korea

Resume : Customization of organic thin film patterns with high functionality has been considered an essential process especially for high-performance micro/nanoscale device applications. In general, for the patterning of functional organic films, there are several essential steps such as coating of hard mask, patterning, etching, and removing of the mask, which can often alter the fundamental properties. Here, we introduce a useful patterning method for thin film positioning, which can both realize selective patterning and exempt the requirement of a subsequent etching step. This advancement is based on spontaneous dewetting property of thin film on the surface with low surface energy. At low temperature, the polymer film can be stabilized and positioned on hydrophilic areas where hydrophobic fluorine-based self-assembled monolayer was not coated. Moreover, we obtained sub-10 nm ultrathin polymer thin film formation by this cold spin-casting (CSC) method. This CSC method may suggest a new way for formation of two-dimensional nanoscale complex pattern customization.

Authors : Sergey M. Karabanov, Dmitry V. Suvorov, Yulia M. Stryuchkova, Gennady P. Gololobov, Viktor S. Gurov, Vladislav S. Loginov, Dmitry Yu. Tarabrin
Affiliations : Ryazan State Radio Engineering University, Ryazan, Russia

Resume : Coatings on the basis of Ni-W alloy are widely used as corrosion-resistant and abrasion-resistant coatings due to high chemical stability, tensile strength and hardness. Traditional method to obtain coatings on the basis of Ni-W binary alloy is electrodeposition. Main problem of coatings on the basis of Ni-W alloy is formation of coating defects in the form of cracks and wedge-like defects significantly decrease functional properties of the coating and being a reason of its delamination. It is practically important to search methods for decreasing of a number of coating defects. The paper has shown results of experimental researches of synthesis of Ni-W alloy coatings by the method of electrochemical deposition from pyrophosphate electrolyte in the mode of direct and pulse current. Data on influence of parameters of the electrochemical synthesis process on characteristics of the deposited coating structure (coating grain size, roughness, characteristic dimension, crack length etc.) and coating microhardness have been obtained. It is found that usage of the pulse mode allows significantly decreasing a number of coating defects. Data on influence of deposition terms on current output, growth rate and chemical composition of coatings have been obtained. Parameters of the electrodeposition mode have been determined when crack-free structure and minimal roughness of coatings are achieved. Electrodeposition modes have been determined when structure of wedge-like defects with high degree of order and orientation is achieved. Obtained results have a practical significance for synthesis of functional Ni-W coatings.

Authors : A. Michel, A. Fillon, G. Abadias
Affiliations : Institut Pprime, UPR 3346 CNRS-Université de Poitiers-ENSMA, Département de Physique et Mécanique des Matériaux, SP2MI, Bld Marie et Pierre Curie, Téléport 2, 86962 Chasseneuil, France

Resume : Understanding the processes at atomic level during thin film growth is of particular relevance to tailor the microstructure and film properties. Monitoring the stress evolution during sputtering with an in situ wafer curvature technique (MOSS) gives valuable information on phase change, dynamical segregation or defect creation. Moreover, when the film adopts a 2D growth mode, interfacial effects manifest more critically : this is the case for Mo/Si multilayers. Mo/Si multilayers, with bilayer thickness L from 5 to 30 nm were grown on Si(001), while varying deposition parameters such as Ar working pressure or bias substrate voltage. In situ measurements of the stress evolution (MOSS) were linked to the growth of an amorphous interfacial layer and to an amorphous-to-crystal phase transition. From ex situ XRD measurements, using the ideal direction "sin²-psi" method, additional information are obtained on the evolution with L of the lattice parameter of crystalline Mo, as well as the main in-plane stress components. Structural characterisation of the multilayers also includes XRR and HRTEM. After the amorphous interfacial layer (~2 nm); a striking feature is the appearance of a transient compressive stress when the Mo transforms to crystalline, followed by the development of a non equi-biaxial tensile stress, that is eventually replaced by the compressive stress due to atomic peening. These features can be attributed to the dynamical segregation of Si during growth.

Authors : Jan Schäfer (1)*, Markus Becker (1), Florian Sigeneger (1), Jorit Gröttrup (2), Daria Smazna (2), Matthias Mecklenburg (3), Yogendra K. Mishra (2), Rainer Adelung (2), Bodo Fiedler (3), Rüdiger Foest (1)
Affiliations : (1) Leibniz Institute for Plasma Science and Technology, Felix-Hausdorff-Str. 2, 17489 Greifswald, Germany; (2) Institute for Material Science, Christian-Albrechts-University of Kiel, Germany; (3) Institute for Polymer & Composites, Hamburg University of Technology, Germany

Resume : The study introduces an innovative application of nanostructured aerographite for the high-speed thermography of an atmospheric pressure plasma jet. The material has been created by conversion of a 3D highly porous ZnO network to a hollow carbon 3D structured network via novel single-step CVD synthesis [1]. The suitability of the application is based on a short response time of aerographite to the temperature changes and on a high infrared emissivity, which equals 1.0. These properties are demonstrated utilizing a radiofrequency capacitively coupled plasma jet operating with argon at atmospheric pressure [2]. The argon gas flows from the plasma jet into the ambient atmosphere where quenching of active species and thermal relaxation occur. The visualization of the thermalization presents a methodological challenge with decreasing relaxation time and concentration of active species. The aerographite surface has been placed in parallel to the gas flow, in lateral distance of few mm. Its surface temperature has been monitored in perpendicular direction using a high speed infrared camera at 600 Hz. Using this technique, a distinct hot spot in the plasma effluent has been discovered. Its existence has been independently proved using laser Schlieren deflectometry (LSD) [2]. [1] M. Mecklenburg at al, Adv. Mater. (2012) 24, 3486. [2] J. Schäfer et al, Eur. Phys. J. Appl. Phys. (2015) 71, 20804.

Authors : I.Saafi1, G. Schmerber2, A. Amlouk1, A.Dinia2, M. Amlouk1
Affiliations : 1 Unité de Physique des dispositifs à Semi-conducteurs UPDS, Faculté des Sciences de Tunis, Université de Tunis El Manar, Tunisie. 2 Université de Strasbourg, CNRS, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), UMR 7504, 23 rue du Lœss, B.P. 43, 67034 Strasbourg Cedex 2, France

Resume : The development of transparent conducting coatings as thin film-electrodes with interesting physico-chemical characteristics like high electron work function, high electron mobility and high transparency, hence, is becoming more relevant. Indeed, to meet these forthcoming requirements, novel alloys or cost-effective preparing techniques are in demand. One of these approaches is focusing on a preparation of ternary oxides by the spray pyrolysis technique. This work deals with some physical studies on SnO2–ZnSnO (TO-ZTO) alloy sprayed nanofilms grown on sapphire substrates at different temperatures (450°C and 600°C). The structural and optical properties were investigated using X-Ray diffraction (XRD), UV visible spectroscopy and Photoluminescence (PL) techniques. XRD results reveal the existence of a mixture of SnO2/ZnSnO3 and SnO2/Zn2SnO4 phases at T=450°C and 600°C, respectively. The structural analysis shows that both phases are polycrystallines. On the other hand, the optical constants (refractive index, extinction coefficient and the dielectric constants) have been obtained by the transmittance and the reflectance data. The optical band gap energy value changed from 3.96 eV down to 3.78 eV as substrate temperature increased from 450°C up to 600°C. The room temperature photoluminescence results reinforce this finding regarding the existence of three phases (SnO2, ZnSnO3 and Zn2SnO4) which is consistent with X-Ray diffraction analysis.

Authors : Hak Ki Yu
Affiliations : Dept. of Materials Science and Engineering and Dept. of Energy Systems Research, Ajou University, Suwon, Korea

Resume : The catalytic activity of transition metal for carbo-hydroxyl molecules (CxHy) have made new technological achievement in graphene growth. For the breakthrough in application of graphene, especially in transistor based electronics, the opening of Dirac-point in graphene is a critical issue. One of the simplest method to open the band-gap at Dirac point is making multi-layer of graphene. However, in this case, the exact positioning or patterning of multi-layer graphene island in 1-layer graphene is not so easy. In this work, we successfully have controlled the number of graphene layer (n-layer) by using Cu-Ni hetero catalyst which has different carbon solubility but has similar lattice structure. Graphene on Ni surface which has higher carbon solubility then Cu tends to form multi-layer of graphene (n >=2), whereas the n is only 1 for the graphene on Cu surface. By patterning the Ni surface using photo-lithography, we can control not only the number of graphene layer but also the position of it. Moreover, to make a flat and high quality graphene surface, we have used extremely flat hetero-catalytic (Ni pattered Cu foil) metal foil using peel-off techniques based on our previous key ideas. Additionally, using magnesium oxide (MgO) layer on Cu surface, we can block the catalytic reaction for the graphene growth, where n=0. As a result, using hetero-structured catalyst (MgO-Cu, Ni-Cu, and Cu), we can control the number of layer from 0 to >=2 easily. This key-idea will be used as a fundamental growth technique in the graphene research society.

Authors : Jau-Yu Chiou, Yu-Wei Hsiao, Jiang-Jen Lin
Affiliations : National Taiwan University

Resume : A series of halogen-free nanocomposites comprising of the exfoliated nanoscale silicate platelets (NSP), organic resins for surface coatings and films was studied. The composite coatings (inorganic nano-clays and organic modifiers) facilitated the resin films for multi-functions of heat and flame-blocking. The nanoscale silicate platelets (NSP) were derived from the exfoliation of natural layered clays in previous works and self-piling into films with a highly regular waved structure and an appreciable volume of air entrapped in between (over 40% in density). The organic modifiers including methylated melamine, phosphorus and water-borne polyurethane were formulated into the coating films for improving the adhesiveness and physical properties. The entrapped air is the main thrust principle for the compositions that retard the heat and flame penetration. The high efficiency of flame-blocking in both of z and x-y axis was demonstrated by coating on brown paper, which ultimately showed their inertness against heat and flame attacked. Layered structures of NSP composites were analyzed by scanning electron microscope (SEM) and the flame test under butane torch was performed in a video, for showing the prevention of flame spread x-y and z-axis flame penetration for over 120 seconds. This remarkable clay nanohybrid coating has a numberless of uses including heat insulator, fireproof devices, gases barrier on transportation, building, aerospace, electronics.

Authors : James A. Behan, Serban N. Stamatin, Md. Khairul Hoque, Guido Ciapetti, Federico Zen, Letica Esteban-Tejeda, Paula E. Colavita
Affiliations : School of Chemistry, CRANN and AMBER Research Centres, Trinity College Dublin, College Green, Dublin 2, Ireland.

Resume : The nitrogenation of carbon materials has been widely studied in recent years due to the applications of these materials in areas such as electrocatalysis, electroanalysis and energy storage. Nitrogen-incorporated amorphous carbon (a-C:N) thin films are attractive materials as these films often possess desirable mechanical properties and corrosion resistance due to the incorporation of nitrogen into the carbon matrix. In this work we synthesized a-C:N thin films with different nitrogen contents via DC magnetron sputtering using different ratios of N2/Ar gas in the plasma during deposition. The films were characterised using a combination of spectroscopic and electrochemical methods including X-ray photoelectron spectrosopy, spectroscopic ellipsometry and electrochemical impedance spectroscopy. Results show that low levels of nitrogenation yield carbon materials with narrow optical gaps and semimetallic character. These materials also display fast electron-transfer kinetics to the outer-sphere hexammine ruthenium(II)/(III) redox couple, suggesting a correlation between bulk optoelectronic properties and electrochemical performance for outer-sphere redox probes. Increasing levels of nitrogenation decrease the metallic character of the films, ultimately yielding materials with optoelectronic properties consistent with disordered cluster aggregates. The bulk properties of the a-C:N films can be easily tuned by controlling the flux of nitrogen gas into the deposition chamber.

Authors : D.V. Sosnin, D.A. Kudryashov, A.M. Mozharov
Affiliations : St. Petersburg Academic University, Khlopina 8/3, 194021 St. Petersburg, Russia

Resume : Titanium nitride is a promising material due to its low resistivity, high hardness and chemical inertness. Titanium nitride can be applied as an ohmic contact for n-GaN and rectifying contact for p-GaN and also as a part of perovskite solar cell. A technology of TiN low temperature rf-magnetron sputtering has been developed. Electrical and optical properties of titanium nitride were studied as a function of the rf-power and gas mixture composition. Reflectance and transmittance spectra were measured. Adhesion and chemical resistance, including resistance to scratching and abrasion were tested. Cross-section and surface SEM image were obtained. 200 nm thin films of TiN with a resistivity of 23.6 µOm cm were obtained by rf-magnetron sputtering at low temperature.

Authors : Siddardha Koneti, Marco S. Rodrigues, Joel Borges, Lucian Roiban, Filipe Vaz, Thierry Epicier, Philippe Steyer
Affiliations : Univ. Lyon, INSA-Lyon, MATEIS UMR CNRS 5510, 21 Avenue Jean Capelle, 69621, Villeurbanne cedex, France; Centro de Física, Universidade do Minho, Campus de Gualtar, 4710 - 057 Braga, Portugal; SEG-CEMUC, Mechanical Engineering Department, University of Coimbra, 3030-788 Coimbra, Portugal;

Resume : Due to their extraordinary properties, nanoparticles (NPs) have been attracting a great interest since their discovery. Noble metal-nanoparticles, and especially gold-nanoparticles (Au NPs), have received an intensive scientific and technological attention as they have unique chemical and physical properties. In particular, interesting optical properties are obtained when metallic NPs (such as Au NPs) are distributed into a dielectric media (e.g., TiO2) as it can be achieved in magnetron-sputtered thin films, followed by post-deposition thermal annealing, owing to the Localized Surface Plasmon Resonance (LSPR) [1] [2]. This effect is closely related to the size, distribution and shape of particles, which thus needs to be quantified in 3D at a nanoscale. In this context, Electron Nano-Tomography (ENT) is a very-well adapted approach [3] and such a study has been performed here in a Cs-corrected Environmental TEM. ENT experiments consist in acquiring tilted series of projections of the object. They were carried out in situ from room temperature to about 600°C in order to better quantify dynamic effects. It was demonstrated that NPs located near the outer surfaces of the film grow significantly more than internal NPs due to the higher atomic mobility. [1] S. Reymond-Laruinaz et al. (2014). Growth and size distribution of Au nanoparticles in annealed Au/TiO 2 thin films. Thin Solid Films, 553, 138. [2] Joel Borges et al. (2016). Broadband Optical Absorption caused by Plasmonic Response of Coalesced Au Nanoparticles Embedded in a TiO2 Matrix. The Journal of Physical Chemistry C, 120, 16931-16945 [3] S. Carenco et al. (2016). The core contribution of transmission electron microscopy to functional nanomaterials engineering. Nanoscale, 8(3), 1260.

Authors : Vilko Mandic, Christelle Nivot, Arnaud Tricoteaux, Philippe Champagne
Affiliations : University of Valenciennes and Hainaut-Cambresis (UVHC), Laboratory of Ceramic Materials and Associated Processes (LMCPA), Boulevard Charles de Gaulle, 59600 Maubeuge, France

Resume : With plethora of various cheap mono-functional anti-corrosive coatings, the questions have been raised regarding their feasibility. Smart coatings recently bring up self-healing, selective- and multi-activity. Yet, they usually utilise complex nanostructural architectures or chemical functionalisation, which is rarely cost-effective. This investigation tries to utilise the cheap wet-chemistry synthesis to from a simple nano-coating. Homogeneous layers of materials, which separately show only average properties, are assembled in multifunctional composites, with the aim to match the level of functionality of the ?smart materials?, yet advantageous in price, scale-up possibility, etc. In contrast to often reported, this concept reposes on dense layer adjecent to substrate to act as a physical barrier. The ordered bonds in dense layer could yield the upgrade of the mechanical properties so the goal is to make it crystalline. The dense layer may not perfectly cover the substrate due to its high surface roughness (also thermal expansion coefficient mismatch), where the second layer is of key importance. Subsequent layer should be tailored to have open-pore porous microstructure but also to remain with reasonable mechanical properties. The pores should serve as a container for infiltration of agent, for example of a standard anticorrosive liquid. Tailoring of the corrosive protection depend on infiltrated agent, while additional functionality can be ensured by adding further layers.

Authors : D. Martínez-Martínez, C. Herdes, Lourdes F. Vega
Affiliations : Center of Physics of the University of Minho, Campus de Azurem, 4800-058 Guimaraes, Portugal; Department of Chemical Engineering, University of Bath. United Kingdom; Gas Research Center and Chemical Engineering Department. The Petroleum Institute. P.O. Box 2533. Abu Dhabi. United Arabs Emirates.

Resume : We present a model for simulating thin film deposition including crystallization processes, within the context of Kinetic Monte Carlo simulations. The model includes a novel crystallization algorithm which modifies the hopping energy barrier depending on geometrical configuration (Geometrical Energy Modification-Crystallization Algorithm, GEM-CA). The problem of “induced order” caused by the application of regular lattices in these types of simulations has been avoided by including two kinds of atoms. The new model allows obtaining both amorphous and crystalline structures, as well as mixed structures (i.e. nanocomposites), depending on the synthesis parameters. A method for the analysis of deposited structures based on its degree of order has been developed. The influence of different deposition parameters such as temperature or composition are discussed, which reproduce the trends experimentally observed.

Authors : Abdelkrim Fedala, Ines Lachebi, and Mohamed Kechouane
Affiliations : USTHB, Faculté de Physique, Laboratoire de physique des matériaux, Equipe Couches Minces et Semiconducteurs, B.P. 32, El Alia, 16111 Bab-ezzouar, Algers, ALGERIA

Resume : We report in this work some results about the effect of annealing process on samples of aluminum thin layer (about 10 nm) deposited by thermal evaporation at room temperature and at a residual pressure about 5.10-6 mbar. The used substrates are corning glass and crystalline silicon wafer oriented (100). Samples with the same thickness of 10 nm are annealed at 580°C just after the deposition without breaking the vacuum at different duration times (from 0,5 to 3 hours). Two samples with thicknesses 5 and 10 nm are annealed during 0,5 hours. The samples are observed by Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM). These observations shows that for the samples annealed at 0,5, 1 and 2 hours the aluminum layer begins to crack. When the annealing duration increases the layer is more and more cracked. For the sample annealed during 3 hours the SEM images shows a formation of homogenous nanoparticles with a mean diameter around 15 nm. The SEM images of the two different thickness samples show that the thinner layer is more cracked than the thicker one. On the other hand we showed that the same annealing process does not lead to the formation of nanoparticles or to the cracked layer if the vacuum is breaked between aluminum deposition and annealing step. This is explained by the well known effect of the oxidation of the aluminum.

Authors : T. Maerten, C. Jaoul, C. Le Niniven, F. Meunier, O. Jarry, P. Tristant
Affiliations : Oerlikon Balzers France & Université de Limoges-SPCTS; Université de Limoges-CNRS-SPCTS; Université de Limoges-CNRS-SPCTS; Oerlikon Balzers France; Oerlikon Metaplas; Université de Limoges-CNRS-SPCTS

Resume : Diamond-Like carbon Coatings could be a promising material for corrosion protection of corrodible substrates like steel due its remarkable chemical inertness properties, its low electrical conductivity, its amorphous and free of grain boundaries microstructure. However, these properties can only be useful in the case of coatings without any spaces for contact between the electrolyte and the substrate to be protected. If not, the non-coated areas will undergo crevice or pitting corrosion depending on adhesion of the DLC. In this work, a comparison between different DLC coating architectures is presented. Actually, multilayered architectures of coating are used to ensure good adhesion of DLC on steel substrates. Nevertheless, most of adhesion layers are columnar and deposited by PVD processes that can generate defects (void, droplet, dust, flake, etc.). The resulting free spaces cannot be filled by the DLC top layer and lead to open channels for electrolyte down to the substrate. Corrosion protection is both evaluated by neutral salt spray test and electrochemical tests including polarization curves and open circuit potential. To conduct and analyze salt spray test, ISO:9227 and ASTM G46 standard are used and surface observations by SEM are performed. Correlation between neutral salt spray and electrochemical tests is discussed to provide an interpretation of the corrosion resistance results.

Authors : B.O. Postolnyi1,2, V.M. Beresnev3, G. Abadias4, L. Rebouta5, J.P. Araujo2, A.D. Pogrebnjak1
Affiliations : 1Sumy State University, 2 Rymskogo-Korsakova st., 40007 Sumy, Ukraine 2IFIMUP and IN-Institute of Nanoscience and Nanotechnology, Department of Physics and Astronomy, Faculty of Science, University of Porto, 687 Campo Alegre st., 4169-007 Porto, Portugal 3V.N. Karazin Kharkiv National University, 4 Svobody Sq., 61022 Kharkiv, Ukraine 4Institut Pprime, Department of Physics and Mechanics of Materials, CNRS - University of Poitiers - ENSMA, 11 Blvd. M. et P. Curie, BP 30179, F86962, Chasseneuil-Futuroscope cedex, France 5Centre of Physics, University of Minho, Alameda da Universidade, 4804-533 Guimarães, Portugal

Resume : Multilayer Transition Metal Nitride CrN/MoN films were produced by physical vapour deposition (Arc-PVD) on stainless steel substrates. Layer thickness varies in range from 20 nm to 1.1 µm with total films thickness up to 14.7 µm. The elemental analysis was performed by energy-dispersive X-ray spectroscopy (EDS). Multilayer microstructure on cross-section samples, as well as morphology of film surface, were analysed with scanning electron microscopy (SEM). Various X-ray diffraction (XRD) methods, including grazing incidence and in-plane were applied to identify phase composition, study coatings structure, evaluate presence of residual stresses, calculate lattice constants and crystallite size. Hardness (H) and elastic modulus (E) were measured by microindentation of samples. For ranking of coatings wear resistance and toughness H values and H/E ratio were used. It was clearly seen that with decreasing of layer thickness the crystallite size also decreases. In its turn the improvement of protective properties of coatings was observed with reducing layer thickness to minimal produced dimensions. Hardness has reached 42 GPa when individual layer thickness was 20 nm.

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Characterization methods at the nanoscale of nano-engineered thin films 2 : J.F. Pierson + T. Belmonte
Authors : T. EPICIER
Affiliations : Univ Lyon, INSA-Lyon, MATEIS, CNRS UMR 5510, F-69621 Villeurbanne, France

Resume : Thin films are today considered as full part functional nanomaterials. During the last decades, applications of quasi two-dimensional nano-engineered coatings and multi-phase / multi-layered thin films have been widely extended in the fields of nanomechanics, biology, tribology or optics. These developments were possible owing to improvements in tailoring innovative approaches. Accordingly, the level of complexity of structures and nanostructures has increased to a point where imaging, metrology and chemical analysis are compulsory for any better understanding, thus optimizing of these fascinating nanomaterials. In this context, advanced electron microscopy provides powerful tools to investigate such features at the desired scale. Focused Ion Beam (FIB) prep techniques help now to take away very well adapted samples for optimized Transmission Electron Microscopy (TEM) studies. Aberration-corrected instruments allow to access almost any desired level of resolution from a spatial and chemical point of view, even in 3D. In situ techniques, either nanomechanical, electrical or environmental solicitation can be used for a better characterization under conditions close to the future using conditions. The purpose of this contribution is to illustrate such approaches, mostly in the case of thin films problematics. Acknowledgements Thanks are due to CLYM ( for access to microscopes in Lyon. This work is partly supported by the French ANR project ‘3DCLEAN’ ANR-15-CE09-0009.

Affiliations : Université de Lorraine, Institut Jean Lamour, Département CP2S, UMR CNRS 7198, Parc de Saurupt, Nancy, F-54011, France.

Resume : Micro and nano-patterning of surfaces is a still challenge in the field of MEMS and NEMS devices assembled via top-down approaches. Consequently, a possible strategy to tackle this problem consists in the development of 3D micro and nano-fabrication processes with high flexibility of use, wide versatility of materials and substrates choice and high deposition rates to process an object in a short period of time. Among the foreseen technologies, atmospheric pressure plasma treatments are relatively low-cost and can be envisaged in a wide range of applications from electronic to medicine. We propose a new process, named Discribe, based on an atmospheric pressure plasma in which a precursor is introduced by means of a nano-capillary. This novel approach allows any end-user to “write/erase” patterns over a surface without resorting to specific and expensive masks. In addition, tridimensional printing can be easily solved by using a moving XYZ stage where the gap between the capillary and the substrate surface can be adjusted on demand. Composite coatings can be deposited alike by adding nanoparticles in the precursor flow. Overall, this new process of additive manufacturing by atmospheric plasma offers an unusually high resolution at low cost. This study demonstrates the possibility to deposit sub-micrometric localized coatings − spots, lines or even more complex shapes – made of amorphous hydrogenated carbon (a-C:H) [1]. [1] Boileau et al., J. Phys. D: Appl. Phys. 49 (2016) 445306

Authors : R. Dedoncker1, B. Braeckman1, N. Martin2, P. Djemia3, L.Belliard4, G. Abadias5, D. Depla1
Affiliations : 1: Department of Solid State Sciences, Ghent University, Krijgslaan 281 (S1), 9000 Gent, Belgium 2: Institut FEMTO-ST, UMR CNRS 6174–Université de Franche Comté − CNRS − ENSMM − UTBM, 15B, Avenue des montboucons, 25030 Besançon Cedex, France. 3: Laboratoire des Propriétés Mécaniques et Thermodynamiques des Matériaux, UPR CNRS 9001, Université Paris-Nord, 99 av.J.B. Clément, 93430 Villetaneuse Cedex, France 4: INSP UPMC, Institut des NanoSciences de Paris, 4 Place Jussieu, 75252 Paris Cedex 05, France 5: Institut P', Département Physique et Mécanique des Matériaux, CNRS − Université de Poitiers − ENSMA, SP2MI, Téléport 2, BP 30179, Futuroscope-Chasseneuil, France

Resume : High-entropy alloys consist of at least 5 different metals in near-equimolar concentrations. A typical example is CoCrCuFeNi. In contrast to the expectation, this material grows as a (111) out-of-plane fiber textured FCC thin film. In the present study, this material is reactively sputtered from a solid target mounted on a two inch magnetron. The influence of oxygen or nitrogen addition to the plasma is investigated. Firstly, the influence of the reactive gas on the discharge voltage, total pressure and deposition rate is studied. In this way, the metallic and the poisoned mode are characterized. Secondly, thin films with a thickness of 500 nm are deposited by adjusting the deposition time. The samples are characterized by XRD, SEM, EDX-WDX and XRR to study the influence of the reactive gas addition on the film morphology, microstructure and texture. The elastic properties are investigated with the aid of PU (Picosecond Ultrasonics) and BLS (Brillouin Light Scattering). A study of the electrical properties of the film is performed by measuring the film resistivity during air exposure by a four probe method as a function of the sample temperature. By cycling the temperature during these latter measurements, film oxidation is investigated. These samples were produced from two different experimental setups, to eliminate chamber dependencies.

Authors : F. Le Normand1, F. Antoni1 , N. Boubiche1, D. Muller1, S. Zafeiratos2, W. Luo2,
Affiliations : 1: ICube, MaCEPV, 23 rue du Loess, 67037 Strasbourg France 2: ICPEES, ECPM, 25 rue Becquerel, 67087 Strasbourg Cedex 2, FRANCE

Resume : Abstract : Graphene thin films on Diamond-like carbon (DLC) films have been obtained on Si or transparent substrates like quartz by pulse laser deposition (PLD) of carbon. Then a transition metal is evaporated (Fe, Co, Ni) at ambient temperature. A subsequent thermal annealing performed in Ultra High Vacuum condition up to 973 K. allows the surface formation of a thin graphitic film on top of the DLC, soon described in Appl. Phys. A, Materials Science & Processing, 71, 433–439 (2000). This film display electrical conductivity combined with high optical transmission and work function, and therefore it could be a possible candidate for transparent electrodes (high conductivity of transparency). Film properties (Thin graphitic layers as well as DLC) has been investigated as a function of many PLD parameters (PLD fluence and time, annealing temperature, nature of the catalyst). The formation of graphene films on top of DLC have been characterized by different techniques including X-ray photoemission, electron-energy-loss spectroscopies, Raman scattering, Nuclar Reaction analysis (NRA).

Authors : Romain Famulok*, Philippe Rodriguez*, Yannick Le Friec**, Jean-Philippe Reynard**, Karen Dabertrand**, Benoit-Noel Bozon***, Sylvie Favier*,**, Yann Mazel*, Emmanuel Nolot*, Bernard Previtali*, Patrice Gergaud*, Fabrice Nemouchi*
Affiliations : * Univ. Grenoble Alpes, F-38000 Grenoble, France CEA, LETI, MINATEC Campus, F-38054 Grenoble, France. ** STMicroelectronics, 850 rue Jean Monnet, BP 16, 38926 Crolles, France *** Applied Materials France, 864 chemin des Fontaines, 38190 Bernin, France

Resume : Using a metal-organic tungsten based precursor, a fluorine-free tungsten thin film has been obtained. The process deposition recipe includes a plasma-enhanced CVD step and ALD cycles. This tungsten thin film can be used as low resistance liner and barrier to fluorine diffusion for several applications in replacement of the classical TiN liner. A set of physicochemical characterizations including XRR, in-plane XRD, WDXRF, plasma profiling time of flight mass spectrometry (PPTOFMS) and SEM/TEM observations has been realized in order to study the W thin film structure and properties. The film is perfectly conformal whatever the structure size tested (from tens of nanometers to micrometers wide). We have also highlighted that the F-free W film exhibits the lowest electrical resistivity phase (α-W) but is not pure. Indeed, in addition to a top surface oxidation, a layer located at the W film / substrate interface is present. This interface layer contains impurities, including C and O, due to ligand decomposition. It might be deposited during the soak step or during the PECVD step. The W liner with thicknesses ranging from 3 to 4 nm has been implemented on PCRAM structures in order to evaluate its impact on contact plug resistivity. First electrical results are promising and demonstrate the interest of using a F-free low resistance W liner. At the aspect ratio studied, the gain in terms of contact plug resistivity is about 20 % compare to the process of reference using a TiN liner.

Authors : Sebastian Gerke 1), Marilyne Sousa 1), Marina Krumova 2), Stefanie Ebert 2), Reinhart Job 3), Barbara Terheiden 2)
Affiliations : 1) IBM Research – Zurich; 2) University of Konstanz; 3) Münster University of Applied Sciences

Resume : The dependence of the morphology of an amorphous silicon (a-Si) film on the deposition technique is known since the late 1970s. Chemical vapor deposition (CVD) supports a non-columnar growth of the a-Si, while physical vapor deposition (PVD) yields a columnar growth including branches. Further, more recent investigations discover an interaction of layers morphology and embedded hydrogen, mainly affecting layer characteristics as e.g. surface passivation capability. Moreover, literature reports the growth of an a-Si layer on crystalline silicon within the very moment of plasma ignition in a CVD process. Morphology depended characteristics as well as the existence of different layers can be observed by indirect characterization methods like growth rate analysis, nuclear resonant reaction analysis and/or Fourier transformed infrared spectroscopy. Until now, a cross-check of these indirect methods by direct investigation, like electron microscopy observations, was not possible, as the morphological effects are on an atomic scale. By comparing different a-Si morphologies in a multi-layer stack, direct observation of an in situ grown layer in the early beginning of a CVD a-Si deposition by tunnel electron microscopy becomes possible. The authors would like to present their latest results and insights emerged by using a sub atomic resolution transmission electron microscope located in the noise-free laboratories of the Binnig and Rohrer Nanotechnology Center at IBM Research-Zurich.

Authors : Jiri Rezek,Jaroslav Vlcek,Jiri Houska,Jiri Capek,Pavel Baroch
Affiliations : University of West Bohemia, Univerzitni 8, 30614 Plzen, Czech Republic

Resume : Densified and highly optically transparent zirconium dioxide films (extinction coefficient of 2 x 10-4 at 550 nm) were prepared by reactive ac magnetron sputtering on a floating substrate in argon-oxygen gas mixtures. We used two unbalanced magnetrons in a closed-field configuration equipped with zirconium targets (100 mm in diameter) driven by a mid-frequency ac power supply producing sinusoidal waveforms of the target voltage and current. The depositions of the films were performed at the repetition frequency of about 85 kHz, the total pressure close to 1 Pa and the average target power densities of 5 – 15 Wcm-2 which are used in industrial ac magnetron sputtering systems. We found that a simple feed-back pulsed reactive gas flow control [1] is very effective also in industrially-demanded reactive ac magnetron sputtering. The method led to a stable, arc-free sputtering process with enhanced deposition rates (up to 84 nm/min), being up to 2.5 times higher compared with the depositions in an oxide mode at the same target power density. We will report on deposition characteristics, mechanical and optical properties of the films and their surface morphology. [1] J. Vlček, J.Rezek, J. Houška, R. Čerstvý, R. Bugyi, Surf. Coat. Technol. 236 (2013) 550.

Authors : Lukas Gröner, Eduart Reisacher, Eberhard Nold, Alexander Fromm, Frank Meyer, Chris Eberl, Frank Burmeister
Affiliations : Fraunhofer IWM Freiburg

Resume : Mn+1AXn phases belong to a group of ternary nitrides or carbides, where M denotes an early transition metal, A denotes mostly a group III or IVA element and X is either nitrogen or carbon. In recent years, an increasing number of investigations on the synthesis and characterization on crystalline Mn+1AXn phases have been published which focus on their suitability for industrial applications, e.g. as protective coatings. Due to the mixture of strong covalent MX bonds and weak ionic MA bonds, these materials often exhibit a high corrosion resistance as well as good electrical conductivity and thermal stability. However, these properties strongly depend on the material*s crystallinity. Ti2AlN MAX-phase thin films were synthetized on various substrates in a reactive sputter mode by a multilayer-deposition of AlN and Ti single layers under variation of the double layer thickness, followed by a subsequent annealing step. The synthesis results were investigated by elemental analysis and electron microscopy. The evolving microstructure with a preferential orientation in the texture was analyzed by polarized Raman spectroscopy and XRD. Besides temperature and annealing time, the double layer thickness turned out to be a key parameter to adjust the orientation and grain size.

Authors : Stefan Mertin, Vladimir Pashchenko, Bernd Heinz, Oliver Rattunde, Gabriel Christmann, Marc-Alexandre Dubois, Sylvain Nicolay, Paul Muralt
Affiliations : EPFL; EPFL; Evatec; Evatec; CSEM; CSEM; CSEM; EPFL 1 Electroceramic Thin Films Group, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, Switzerland 2 Evatec AG, Hauptstrasse 1a, CH-9477 Trübbach, Switzerland 3 CSEM, Rue Jaquet-Droz 1, CH-2002 Neuchâtel, Switzerland

Resume : Partial substitution of aluminium by scandium in the wurtzite structure of aluminium nitride (AlN) leads to a large increase of the piezoelectric response by more than a factor of 2. Therefore, aluminium scandium nitride (ASN) thin films attracted much attention to improve piezoelectric MEMS devices such as RF filters, sensors, micro actuators and energy harvesting devices. In this work, process-microstructure-property relationships of ASN thin films containing up to 40% Sc were investigated. Like AlN thin films, ASN films are as well sputter deposited at 300–350 °C with pulsed DC or RF powered magnetrons. In order to achieve piezoelectric active films with a high Sc concentration, the influence of the process parameters on the film structure, the intrinsic stress and the piezoelectric response was carefully investigated. X-Ray diffraction (XRD) was used to confirm c-axis textured film growth. Such films exhibit for the (002) ASN peak a rocking curve of around 1.3–2° (FHWM). The films were further analysed by electron microscopy and the Sc content was determined by energy-dispersive X-ray spectroscopy (EDX). A good compositional homogeneity in the range of 0.5–1 at% was achieved between border and centre of 200-mm wafers. So far, we obtained ASN films with transversal and longitudinal piezoelectric coefficients up to e31,f = -2.37 C/m2 and d33,f = 10.1 pm/V, respectively. This corresponds to films with more than twice as large piezoelectric coefficients as AlN.

Authors : Anne-Catherine Probst 1, Thorsten Döhring 1, Florian Emmerich 1, Manfred Stollenwerk 1, Franziska Riethmüller 1, Veronika Stehlíková 2, Mingwu Wen 3, Laura Proserpio 4
Affiliations : 1: Aschaffenburg University of Applied Sciences, D-63743 Aschaffenburg, Germany; 2: Czech Technical University in Prague, CZ-16627 Prague 6, Czech Republic; 3: Institute of Precision Optical Engineering, Tongji University, Shanghai 200092, China; 4: Max-Planck-Institute for Extraterrestrial Physics, D-85748 Garching, Germany.

Resume : Reflective mirror coatings made of iridium are often used in X-ray telescopes investigating astronomical sources at photon energies below 10 keV. Due to the reduced mirror thickness (< 1 mm) for next generation X-ray observatories, enhanced coating properties are required. In particular, low coating stress is needed to avoid unwanted deformations of the initial precisely shaped mirror substrates, which would affect the angular resolution of the telescope. The development of thin iridium films deposited using an RF-magnetron sputtering technique presented here is focused on the influence of the substrate material quality and the deposition parameters on the thin film properties. XRD, XRR and AFM characterization methods have been used. Correlations between coating density, surface micro-roughness, crystalline structure of the iridium layers and the expected reflectivity as well as stress-induced deformation of the X-ray mirror will be presented and discussed.

Authors : T.C. Rojas, S. Domínguez-Meister, M. Brizuela, J.C. Sánchez-López
Affiliations : Instituto de Ciencia de Materiales de Sevilla (CSIC-Univ. Sevilla), Sevilla, Spain; Instituto de Ciencia de Materiales de Sevilla (CSIC-Univ. Sevilla), Sevilla, Spain;TECNALIA, Donostia-San Sebastián, Spain; Instituto de Ciencia de Materiales de Sevilla (CSIC-Univ. Sevilla), Sevilla, Spain;

Resume : Multilayered Cr0.50Al0.50N and Cr0.51Al0.46Y0.03N coatings were deposited on M2 and 316 steel substrates and heated to 1000 ºC in air for 2 h to study their oxidation mechanism and thermal stability. X-ray diffraction, glow-discharge optical emission spectroscopy and transmission electron microscopy coupled with spatially resolved microanalysis techniques are used to investigate the nanostructure, constituent phases and chemical elemental distribution of the as-prepared and oxidized samples. The reactive element effect of Y is confirmed but differs from the typical observed in alloys. The interdiffusion of substrate elements plays an important role in the oxidation process influencing the corrosion products. The presence of yttrium retards the iron outward diffusion by forming oxides in M2 and yttrium nitride in 316 steels. The microstructural analysis determined that yttrium migrates to the grains and interface of the oxide scale and to the nitride column boundaries.

Authors : J. Montero, Y.-X. Ji, C. G. Granqvist, G. A. Niklasson
Affiliations : J. Montero - Institute for Energy Technology, P.O. Box 40, NO-2027 Kjeller, Norway Y.-X. Ji; C. G. Granqvist; G. A. Niklasson - Department of Engineering Sciences, The Ångström Laboratory, Uppsala University,P. O. Box 534, SE-75121 Uppsala, Sweden

Resume : Particulate films consisting of thermochromic vanadium dioxide (VO2) have been obtained by reactive magnetron sputtering onto In2O3:Sn coated glass substrates. These films consist of VO2 particles of adequate size to cause light scattering—and hence diffuse transmittance—in the visible region. When these films are heated up above the temperature at which the thermochromic transition takes place, the particles switch from a semiconducting to a metallic state, thereby affecting the overall scattering properties. In this work, layers consisting of particles of different shapes and sizes have been studied by scanning electron microscopy, atomic force microscopy and optical spectrophotometry. The optical properties of the films, including the spectral absorption and scattering coefficients, have been studied below and above the transition temperature. In addition, the experimental optical properties have been reconciled with a semi-quantitative model based on Lorentz-Mie theory and the Grenfell-Warren approximation.

Surface modification/functionalization : Gerry van der Kolk + Peter Panjan
Authors : Rostislav Daniel, Christian Mitterer, Jozef Keckes
Affiliations : Montanuniversität Leoben, Montanuniversität Leoben, Montanuniversität Leoben

Resume : The ability of most hard materials to deform inelastically is usually rather limited since the activation of dislocation glide on most slip systems in hard nanocrystalline ceramic materials requires much higher stress than that for brittle fracture along grain boundaries of a low cohesive energy. On the contrary, materials with enhanced plasticity are usually not very strong. An enhancement of the material fracture toughness without compromising its strength is thus rather challenging. We will demonstrate various innovative material design strategies for fracture toughness enhancement of brittle ceramic nanostructured materials, which rely on a variation in material microstructure and mechanical property depth-distributions, and dedicated grain-boundary and interface design. The film characterization in terms of stiffness, fracture stress and toughness was based mainly on in-situ micromechanical testing of microcantilever beams prepared by focused ion beam milling. Besides strategies to enhance fracture toughness by transformation toughening, coherency strain or intrinsic compressive stress, the main focus will be on microstructural design of thin films to control crack propagation. The microstructure- and property-dependent mechanisms controlling crack propagation (e.g. deflection by weak interfaces or crack path tortuosity) with subsequent toughness enhancement will be discussed in detail for various material combinations (hard/soft crystalline/amorphous and crystalline/crystalline materials). Special attention will be paid to nanocrystalline materials with sculptured chevron-like microstructure, where crack propagation is inhibited by deflection of cracks at the grain boundaries and/or interfaces between stiff and elastic constituents. In this way, even common nanocrystalline brittle materials may exhibit considerably enhanced plasticity and fracture toughness achieving values more than 150% of their monolithic counterparts with columnar microstructure.

Authors : Qi Tianjiao,Wang Hui , Wang Lin, Yang Fang
Affiliations : Institute of Chemical Materials China Academy of Engineering Physics

Resume : Transparent conductive films (TCFs) is high transparency in visible light(λ=380~780nm)with nearly metallic conductivity. They are important materials and represent more than 50% in functional films. In this paper, highly conductive and transparent TCFs of carbon nanotubes were fabricated by incorporating Nafion® into carbon nanotubes (CNTs) layers. The transparency and electrical conductivity properties of the CNTs/Nafion® thin films were significantly improved by the 3,4-ethylenedioxythiophene (EDOT) incorporation. Conductive carbon nanotubes/Nafion® (CNTs/Nafion®) composites are prepared based on filtration technology. CNTs are first dispersed in ethanol mixed with different amounts of Nafion® and then driven by ultrasonic. From these mixtures CNTs/Nafion® composites were dipped in EDOT. The dispersion of CNTs/Nafion® is characterized by infrared spectroscopy, scanning electron microscopy and UV–vis spectra. When applying adequate preparation conditions, CNTs are well dispersed and homogeneously incorporated in the Nafion®. Using the developed process, CNTs/Nafion® thin films that are uniform and the dispersion of CNTs with Nafion® connected with one another to form an interweaving films and highly transparent have been fabricated. The resistivity and optical transmittance of CNTs/Nafion® with EDOT thin film were 82 KΩ/□ and over 69% with optimum condition when the volume of CNTs/Nafion® was 0.3mL and the ratio of Nafion® was 2.5%. With the optimization of the composition of Nafion® composite, CNTs/ Nafion® thin films might potentially offer better or comparable performances as the conductive oxides.

Authors : Wenjia Shi, ,Kun Tian,Chungang Guo, Guo-an Cheng, Xiaolin Wu, Ruiting Zheng
Affiliations : College of Nuclear Science and Technology,Beijing Normal University,Beijing, China, 100875

Resume : Polyimide (PI) is one of the most popular polymers due to its outstanding physicochemical properties, such as thermostability, corrosion resistant, radiation resistant, chemical stability and so on. These unique properties make PI have wide applications in electronics, automotive and aerospace industries. However, it’s hard to deposite metal film on PI film, which is unfavourable for PI film to use in flexible electronic device. Compared with other surface coating technology, ion implantation is a idea mothod for the surface modification of PI film. In this paper, different ions are used to implant into the PI film. By changing the energy and dosage of ions, we investigate the zeta potential and surface tension variation of PI film implanted by H、He、C、N、Fe、Ti、Zr and Hf ions. The influence of implanted ions on the physicochemical properties of PI is analyzed. It is found that the surface zeta potential of ion implanted PI film has close relationship with surface lewis acidity γL+, which can be use to adjust the surface physicochemical properties of PI film. By changing the surface zeta potential with Fe ion implantation, we successfully realize the surface patterning of nano particles on PI films.

Authors : Sang-Jin Lee, Sung Hyun Kim, Mac Kim, Tae-Woon Kang, Han-Ki Kim, Seong Keun Cho, Dong Seok Ham, Yong Suk Yang, Jae Heung Lee
Affiliations : Sang-jin Lee, Sung Hyun Kim, Mac Kim, Tae-Woon Kang, Seong Keun Cho, Dong Seok Ham, Jae Heung Lee : Korea Research Institute of Chemical Technology ; Sung Hyun Kim, Mac Kim, Yong Suk Yang : Pusan National University ; Han-Ki Kim : Kyung Hee University

Resume : Multi-functional fluorocarbon plasma polymer thin films are fabricated on a large-area polyethylene terephthalate substrate using continuous roll-to-roll sputtering with a 700-mm film width. Carbon/polytetrafluoroethylene composite target is used for the mid-range frequency sputtering for the first time. They exhibit water-repelling surfaces to preventing wetting and to remove contamination. In addition, plasma polymer thin film shows high optical transparency because they have amorphous structure and relatively low optical constants. The maximum optical transmittance of the fluorocarbon thin films with a carbon concentration of 1 wt% is 93.27% at a 550 nm wavelength. The cross-linked carbon structure enhances the hardness and modulus of the fluorocarbon plasma polymer thin films. Surface hardness of the fluorocarbon plasma polymer thin film increases from 0.58 GPa (Carbon 0 wt%) to maximum 6.9 GPa when carbon or inorganic materials are incorporated into the PTFE composite target. The outer bending test shows remarkable mechanical flexibility characteristics with a minimum bending radius of 3 mm and excellent cyclic fatigue resistance. From these results, we confirm that a high hardness fluorocarbon thin film with high hydrophobicity, transparency and flexibility can be fabricated via mid-range frequency roll-to-roll sputtering.

Authors : Camila Honorato-Rios, Jan Lagerwall
Affiliations : University of Luxembourg, Physics & Materials Science Research Unit, Experimental Soft Matter Physics Group

Resume : Cellulose nanocrystals (CNCs), nanorods produced by acid hydrolysis of cellulosic sources, are emerging as a new class of functional biomaterial. CNCs present a broad range of uses, for example in composites, cosmetics, security paper and medical devices [1]. The fascinating ability of CNCs to self-organize into a cholesteric liquid crystal phase, with a helical arrangement of the nanorods, is attracting substantial interest across different research fields [2]. It is important from an applied point of view since this arrangement gives a photonic band gap to the final dried CNC films, but also from a fundamental soft matter physics perspective, as many details of the CNC liquid crystal formation are far from being understood. A critical problem from an analytical, and likely also from an applied perspective, is the high length polydispersity of as-produced CNC samples. In this study, we introduce a method for fractionating the CNC nanorods, utilizing the spontaneous phase separation between isotropic and liquid crystalline phases, allowing us to narrow down the length distribution. The aspect ratio (length/diameter) has a strong effect on the period of the cholesteric helix, affecting the iridescent colors appearing in dried CNC films. We believe that a reduced polydispersity will allow us to better control the color of the finally dispersed films, compared to the natural polydisperse samples that are now being used in the community. We present how this affects the self-assembly process, and consequently the color formation in such bio-derived structural films. [1] J.H. Park et al., ChemPhysChem, 15, 7, pp. 1477-1484 (2014) [2] Lagerwall, J. P. F. et al. Cellulose nanocrystal-based materials: from liquid crystal self-assembly and glass formation to multifunctional thin films. NPG Asia Mater. 6, e80 (2014).

Authors : D. Craciun1, D. Pantelica2, P. Ionescu2, B. S. Vasile3, D. Cristea4 and V. Craciun1
Affiliations : 1National Institute for Lasers, Plasma and Radiation Physics, Magurele, Romania; 2Horia Hulubei National Institute for Physics and Nuclear Engineering, Magurele, Romania; 3Polytechnic University Bucharest, Bucharest, Romania; Transilvania University, Brasov, Romania

Resume : There are many important applications for thin films in areas where there is a strong radiation field. It has been recently showed that thin films which are nanostructured would behave differently under irradiation than polycrystalline or single crystal films. The absence of a relatively long-distance order allows for very short diffusion lengths of irradiation generated defects towards grain boundary regions that act as sinks. Therefore, the structure and properties of such thin films should not be strongly affected by exposure to radiation. Also, dislocations could not exist in very small grains. Therefore, the increase of mechanical hardness after irradiation caused by the generation of arrays of dislocations that will become entangled and therefore immobile, could not be observed in these nanostructured films. To investigate in detail the radiation effects on properties and structure of such materials we used the Pulsed Laser Deposition (PLD) technique to grow nanocrystalline or amorphous thin films from inexpensive targets. By simply changing the deposition parameters, films possessing different chemical compositions and/or structures could be readily obtained. The effects of 800 keV Ar and 1 MeV Au ions irradiation on the microstructure, surface morphology and chemical composition of nanostructured ZrN thin films were investigated and the results compared to those obtained on polycrystalline or single crystal materials. Nanoindentation results clearly showed a significant decrease of hardness and Young modulus in irradiated ZrN films from the initial 35 GPa and 270 GPa to 15 and 160 GPa, respectively.

Authors : Corneliu Sarbu
Affiliations : National Institute of R&D for Materials Physics, Magurele, Romania

Resume : The necessity of providing direct microstructure evidence for the validity of the so-called colossal carbon supersaturation mechanism [1] as applied to the surface carburization of Inconel-718 (IN-718) superalloy [2] triggered the present research. We will present new microstructure findings revealing the nanostructuration of the uppermost surface layer of IN-718 alloy submitted to gas-carburization processing at low-temperature (< 600°C) by the standard procedure invented by Swagelok Co. Ltd. (USA) [3]. Our new results are showing that the mechanism of paraequilibrium diffusion of C atoms in the crystal lattice interstitial positions, up to colossal carbon concentrations and avoiding the carbides formation (LTCSS) is not the true mechanism of IN-718 surface properties modification. Instead, the nanostructuration of the alloy surface layer is revealed, due to the phase instability of initial surface grains in carburization gas atmosphere, an effect which probably occurs also in other similarly processed alloys. Some of the nanostructure features observed by means of HR(S)TEM and EELS were already communicated (see abstracts at [4]), but a comprehensive presentation of our research data will be done herewith. [1] Cao Y, Ernst F, Michal G, Acta Mater 2003; 51, p.4171 [2] Sharghi-Moshtaghin R et al, Metall Mater Trans A, 2010; 41A, p.2022 [3] Collins S and Williams P, Advanced Materials & Processes / September 2006, p.32 [4]

Nanostructured coatings or nano-engineered thin film architectures 1 : Ulf Helmersson + M. Fenker
Authors : Ulf Helmersson, Rickard Gunnarsson, Sebastian Ekeroth, Sadegh Askari, Nils Brenning
Affiliations : Department of Physics, Linköping University, SE-581 83 Linköping, Sweden

Resume : We generate nanoparticles (NPs) using high-power pulsed hollow-cathode sputtering, yielding high productivity and simultaneously excellent control over NPs size and size distribution. The use of the high-power pulses is key to the success of the process, since it provides an efficient ionization of the sputter-ejected atoms. The positive metal ions are very effectively trapped on growing negatively-charged NPs, since NPs are negatively charged in a plasma. A range of materials has been synthesized including Fe, Cu, Ti, Ag, Mo, In and Zn. By adding a reactive gas to the process NPs containing Ti-O, Ti-N, Zn-O and In-N has been synthesized. Several process parameters were identified to affect the size, size distribution, shape and structure of the nanoparticles. These parameters include pulse power, pulse frequency, sputtering gas composition, gas pressure and geometry of the setup. By tuning these parameters, the nanoparticle size can range from a few nm to more than 250 nm in diameter. To fully utilize the synthesized NPs in applications, they often need to be positioned or assembled into complex architectures including nanowires (NWs), pillars, and surface patterns. Since the NPs are negatively charged electrostatic fields can be utilized for this purpose. For magnetic NPs, externally applied magnetic fields make it possible for the NPs to self-assembly into cross-linked NWs, reaching many micrometers in length while only one NP wide (20-60 nm) in the individual NW.

Authors : Guillaume Naudin†*, Karima Bouamama*, Stéphane Delalande*, David Grosso†, Cédric Boissière†, Marco Faustini†.
Affiliations : †Chimie de la Matière Condensée de Paris, UMR UPMC-CNRS 7574, Université Pierre et Marie Curie (Paris 6), 4 place Jussieu, 75231, Paris, France; *PSA Peugeot Citroën, Direction Scientifique, Centre technique de Vélizy, route de Gisy, 78140 Vélizy-Villacoublay.

Resume : Herein we report the development of large scale, antireflective and anti-fogging coatings applied on windshields for automotive industry. Sol-gel based coatings were optimized to fulfill the strict requirements of a car environment. We showed that the pollution rate is a critical point to ensure a sustainable antifogging coating. The “fog effect” can be explained in terms of light scattering due to the formation of water microdroplets onto colder substrates. In most of the papers related to fogging, the macroscopic optical effect is simply associated to the static contact angle of water on the surface. In our work, we rely the macroscopic opacification to a microscopic observation of the nucleation, growth and eventually coalescence of microdroplets onto functional thin films. Computational models based on the Mie theory were then applied to support the experimental results. Interestingly, superhydrophilic TiO2 coatings are not efficient when applied in polluted environments. XPS measurements were performed to explain the role of pollutants accumulation onto the sol-gel layers. The effect of surface energy was further investigated by using other sol-gel coatings exhibiting controlled hydrophilicity/hydrophobicity ratio. Finally, a pre-industrial demonstrator on laminated glass was fabricated by dip-coating. The final material is able to combine the enhanced anti-fogging properties with the other requirements such as anti-reflectivity, colorless and mechanical stability.

Authors : Evangelia Dislaki, Jordi Sort, Eva Pellicer
Affiliations : Departament de Física, Universitat Autònoma de Barcelona, E08193 Bellaterra, Spain; Institució Catalana de Recerca i Estudis Avançats (ICREA) and Departament de Física, Universitat Autònoma de Barcelona, E08193 Bellaterra, Spain; Departament de Física, Universitat Autònoma de Barcelona, E08193 Bellaterra, Spain

Resume : The scarcity of raw elements and the environmental implications of employing hazardous materials in technology have intensified the demand for sustainable and cost-effective alternatives. The Fe–Cu system presents an attractive option due to its wide availability, eco-friendliness and highly tunable magnetic properties. Among the various methods utilized to produce metallic films, electrodeposition is an appealing technique due to its low cost, simple set-up, operation in ambient pressure, fast deposition rates on a variety of substrate geometries and ability to grow fairly thick, homogeneous coatings. Existing literature on electrodeposited Fe–Cu films, however, is limited due to the immiscibility of Fe and Cu and the tendency to form oxides/hydroxides during deposition. Furthermore, film properties depend heavily on fabrication method and experimental conditions. In this work, FexCu1-x continuous films with minimized oxygen content were deposited over a wide composition range (0≤x≤86) from three electrolytes where the complexing agent was altered. The effect of electrolyte composition and plating parameters on the stoichiometry, morphology, structure and magnetic properties of the films was investigated. In a subsequent step, hierarchically porous FeCu films were produced using electrodeposition through colloidal templates (with nanospheres of 200nm, 350nm and 500nm) with a focus on the effect of nanosphere size network characteristics on wettability and magnetic behavior.

Poster session 2: Biological Characteristics of Biomaterials and Thin Films and Related Materials : M. Fenker + Philippe Steyer
Authors : Mariya Khokhlova, Sara Bouhout, Wilfrid Prellier, Adrian David, Karim Boumédiene
Affiliations : Mariya Khokhlova, Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 Bvd Maréchal Juin, 14050 Caen Cedex, France; Sara Bouhout, Laboratoire BioConnect, Université de Caen Normandie, CHU Niveau 3, 14032 Caen Cedex, France; Wilfrid Prellier, Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 Bvd Maréchal Juin, 14050 Caen Cedex, France; Adrian David, Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 Bvd Maréchal Juin, 14050 Caen Cedex, France; Karim Boumédiene, Laboratoire BioConnect, Université de Caen Normandie, CHU Niveau 3, 14032 Caen Cedex, France;

Resume : Stem cells are extensively studied due to their unique properties and great potential in biomedical applications [1]. Thanks to a variety of biological responses, metal-oxide coatings are widely used for interacting with stem cells [2, 3]. A very limited number of oxides have however been studied, and mechanism of the cell-material interaction is still not completely clear. Here, oxides thin films, that are well-known for their electronic properties, are deposited on substrates using the pulsed laser deposition (PLD) technique. Bone marrow mesenchymal stem cells were cultured on the surfaces of thin films and their adhesion, proliferation and differentiation were evaluated as a function of the growth conditions, thickness of the films, surface roughness and morphology. These results will be of a great clinical significance, in particular, in the field of regenerative medicine. M.K. thanks support from Normandie Université for her PhD fellowship. Partial support from project Emergence Normandie, and the FEDER are also acknowledged. References: 1. Bianco, P., Robey, P.G., 2001. Stem cells in tissue engineering. Nature 414, 118–121. 2. Gittarda, Sh. D., Perfect, J. R., Monteiro-Riviere, N. A., Wei, W., Jine, Ch., Narayan, R.J., 2009. Assessing the antimicrobial activity of zinc oxide thin films using disk diffusion and biofilm reactor. Applied Surface Science 255, 5806–5811. 3. Zhang, S., Sun. J., Xu, Y., Qian, S., Wang, B., Liu, F., Liu, X., 2012. Biological behavior of osteoblast-like cells on titania and zirconia films deposited by cathodic arc deposition. Biointerphases 7, 60–70.

Authors : Jung-Dae Kwon, Woo Jae-Lee, and Se-Hun Kwon
Affiliations : Korea Institute of Materials Science, Pusan National University, and Pusan National University

Resume : The stainless-steel based bipolar plate is one of key component of recent polymer electrolyte membrane fuel cells. Due to the low electrical conductivity and insufficient corrosion resistance of stainless-steel, the adoption of coating process is essential for the efficient protection. Despite of the extensive efforts, critical challenges still remain in finding an adequate protective coating material and method, which satisfies the strict requirements. Here, we demonstrate that a high degree of corrosion protection and electrical conductivity of stainless-steel 316L (SS316L) based bipolar plate can be achieved by simply adopting ultrathin (25~67 nm) plasma-enhanced atomic layer deposition (PEALD) of TiN thin films. For this, we carefully evaluated two types of TiN protective coatings prepared by PEALD using tetrakis-dimethylamido-titanium (TDMAT) and titanium tetrachloride (TiCl4) precursors in environments simulating the bipolar plate situation. Regardless of the precursor types, the adoption of PEALD-TiN on SS316L exhibited great improvements in the electrical conductivity and corrosion resistance. Noteworthy, TiN thin films using TDMAT exhibited an excellent corrosion resistance (<1 μA/cm2) than that using TiCl4 precursor. A systemic structural, compositional, and electrochemical analyses reveals that ~5nm-thick ultrathin amorphous interfacial layer, formed when TiN thin films were prepared using TDMAT, played a key role in the corrosion protection. Furthermore, TiN thin films using TDMAT greatly lowered the interfacial contact resistance of SS316L.

Authors : Ha-Linh Thi Le1, 2, 3, Jacek Goniakowski1, 2, Claudine Noguera1, 2, Alexey Koltsov3, and Jean-Michel Mataigne3
Affiliations : 1CNRS, UMR7588, Institut des Nanosciences de Paris, F-75005 Paris, France 2Sorbonne Universités, UPMC Univ Paris 06, UMR7588, INSP, F-75005 Paris, France 3ArcelorMittal Maizières Research, voie Romaine, F-57280, Maizières lès Metz, France

Resume : Adhesion at alumina/zinc interfaces is one of the key issues in steel manufacturing industries. Indeed, while enrichment in elements, such as Al, improves the strength of new steel grades, the selective oxidation of Al may lead to the formation of a quasi-continuous alumina film at the steel surface, which dramatically reduces Zn adhesion strength. It has been shown that transition metal buffers considerably enhance adhesion of the weakly interacting alumina/zinc interface. However, oxidation of such metal buffers has an overall detrimental effect. In the present study, we consider more complex, stainless steel buffers at the alumina/zinc interface. The buffers consist of several metals (M = Cr, Fe, and Ni) and/or of their oxides depending on oxygen conditions and are represented by the corresponding sequence of interfaces. We performed ab-initio simulations to calculate interface and adhesion energies of all interfaces between each two materials. Monte Carlo Metropolis simulations were employed to find the most stable interface sequences in the complex buffer. We analyze the spatial distributions of materials and interfaces in the complex buffers and identify points of weakest adhesion. Our results clearly show that regardless the oxidation conditions, stainless steel buffers produce good adhesion properties which make them promising candidates to improve the adhesion of Zn coatings in the case of Al-enriched steel grades.

Authors : Gabriela Ciobanu (1), Maria Harja (1), Octavian Ciobanu (2)
Affiliations : (1) “Gheorghe Asachi” Technical University of Iasi, Faculty of Chemical Engineering and Environmental Protection, Prof. dr. docent Dimitrie Mangeron Rd., no. 63, 700050, Iasi, Romania; (2) “Grigore T. Popa” University of Medicine and Pharmacy, Faculty of Medical Bioengineering, Universitatii Str., no. 16, 700115, Iasi, Romania

Resume : Because most of the biological reactions take place at the surface level, the implant surfaces play an important role in tissue engineering. Modification of the structure and surface chemistry of an implant can be achieved by various methods, the most commonly used being coating of the implant’s surface by biocompatible layers. Surface modification of titanium implants for bone contacting applications is a very active field of research in tissue engineering. In this research, the hydroxyapatite-collagen-silver coatings have been deposited onto titanium implants by a combined method involving hydroxyapatite/collagen electrochemical deposition, combined with silver ions reduction and in-situ crystallization processes on titanium surface. The electrolytic processes implies the nucleation and growth of hydroxyapatite crystals on the surface of the titanium implant in a simulated body fluid under physiological conditions of pH and temperature, applying a constant current for different periods of time. The collagen has been used to modify titanium surfaces in order to enhance their bioactivity. The silver incorporation into hydroxyapatite coatings is an alternative that can provide good antibacterial properties of these coatings. The morphology, composition and phase structure of the hydroxyapatite-collagen-silver coatings were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX) and X-ray diffraction (XRD).

Authors : 1. Nasrin Banu* 2. B. N. Dev 3. Surendra Singh 4. S. Basu 5. B. Satpati 6. A. Roy
Affiliations : 1,2: Department of Materials Science, Indian Association for the Cultivation of Science, 2A & 2B Raja S. C. Mullick Road, Jadavpur, Kolkata 700032, India. 3,4: Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085, India. 5: Surface Physics and Material Science Division, Saha Institute of Nuclear Physics, 1/AF, Bidhannagar, Kolkata 700064, India. 6: Microelectronic Research Center, The University of Texas at Austin,10100 Burnet Road, Bldg 160, MER 1.606J, Austin, Texas 78758, USA.

Resume : There is a theoretical prediction that normal ferromagnetic fcc cobalt, when compressed to a high density, is likely to have a nonmagnetic phase[1]. In a polycrystalline thin film, the presence of compressive stress can lead to an increase of material density [2]. We have searched for a high density nonmagnetic phase of cobalt in a polycrystalline cobalt thin film and we have succeeded in obtaining the experimental evidence of formation of high density (HD) nonmagnetic cobalt[3]. We have prepared a 25 nm cobalt (Co) thin film on HF etched clean Si(111) at room temperature under high vacuum by e-beam evaporation. We then exposed the film to air due to which about 3 nm cobalt oxide forms on the top of the film. After a sufficiently long time we have carried out X-ray reflectivity (XRR) and polarized neutron reflectometry (PNR) experiments at Bhabha Atomic Research Centre, Mumbai, India. The PNR experiment is repeated at Oak Ridge National Laboratory, Oak Ridge, USA and we have obtained the same results with better precision due to large neutron flux. From XRR fit shown we observed a very high density (HD) layer (high scattering length density) of cobalt at the Co/Co-oxide interface and at the Co/Si interface. Only after considering these two high density layers we get the best fit to the XRR data. From PNR we have corroborated the existance of these HD layers and additionally the PNR data fit shows that these high density Co layers have nearly zero magnetic moment. Cobalt in the mid depth region of the film i.e, between these two high density layers has normal density and magnetic moment. Rutherford back scattering spectrometry experiment has ruled out the presence of any element of higher atomic number than Co. This has confirmed that the HD material is indeed Co. Further we have carried out planar TEM, XTEM, HRTEM, HAADF, EDS, EELS measurements. All these results confirm the formation of high density cobalt within the Co thin film and shows that this HD phase of Co has an fcc lattice structure. From HRTEM in planar view we get an fcc lattice constant of Co which corresponds to 30% of volume reduction (density enhancement) compared to normal Co. Theory predicts an fcc nonmagnetic Co with 1.4 times density of normal hcp cobalt [1]. Our observed HD Co has a density in the range of 1.2-1.4 times the normal Co density. Further results on the dependence of nonmagnetic HD Co formation on the film thickness, capping and substrate will be presented. References: [1] S. F. Matar et al, Phys. Rev. B 75, 245109 (2007). [2] E. Chason et al, Phys. Rev. Lett. 88, 156103 (2002). [3] Nasrin Banu, Surendra Singh, B. Satpati, A. Roy, S. Basu, P. Chakraborty, Hema C. P. Movva, V. Lauter and B.N. Dev, Scientific Reports (in press).

Authors : J. LOUWSMA (a,b), S. JOLY (a), J.-F. LUTZ (b), D. CHAN-SENG (b)
Affiliations : (a) PSA Groupe, Site Vélizy, Chemin de Gisy, 78943 Vélizy-Villacoublay, France (b) Université de Strasbourg, CNRS, Institut Charles Sadron, F 67000 Strasbourg, France

Resume : Fiber-reinforced composite materials find applications in a wide range of fields such as automotive industry for the development of lightweight vehicles [1]. While such materials could provide enhanced mechanical properties, poor polymer matrix-fiber interactions could be detrimental. Various approaches were envisaged to overcome this issue through the treatment of the fibers or addition of agents promoting an enhanced dispersion of the fibers in the polymer matrix [2]. Here supramolecular interactions are being exploited. Sequence-defined oligomers based on amino acids and spacing units were prepared by solid-phase synthesis [3] using phenylalanine as amino acid to promote interactions with aramid fibers. A library of sequence-defined oligomers was synthesized to identify the structural features necessary to obtain compatibilizers leading to fiber-reinforced composite materials of high performances. Their thermal behavior and adsorption on aramid fibers were investigated to evaluate their potential viability to the processes used in the automotive industry and capability to promote compatibilization. 1. (a) Brosius, D., SPE Automotive Composite Conference: proceedings of a conference, 2003,1-7; (b) Chopade S.B. et al., Int. j. innov. res. sci. eng. technol., 2015, 4(1), 18801-18808 2. (a) Saheb D. N et al., Adv. Polym. Technol. 1999, 18, 351-363; (b) Mukhopadhyay S. et al., J. Thermoplast. Compos. Mater. 2003, 16, 479-495 3. Chan-Seng D. et al., ACS Macro Lett. 2014, 3, 291-294

Authors : L. Major -1, J. M. Lackner -2, M. Kot -3, B. Major -1
Affiliations : 1- Institute of Metallurgy and Materials Science, Polish Academy of Sciences, Cracow, Poland; 2- JOANNEUM RESEARCH –Materials, Institute for Surface Technologies and Photonics, Niklasdorf, Austria; 3- Laboratory of Surface Engineering and Tribology, Faculty of Mechanical Engineering and Robotics, AGH University of Science and Technology, Cracow, Poland

Resume : Much research has been devoted to exploring potential advantages of a thermoplastic matrix for composite materials. Such matrix is polyaryletheretherketone (PEEK) which exhobits exceptional properties due to its semicrystalline character and the molecular rigidity of its repeating units. PEEK materials are semicrystalline aromatic polyesters with excellent mechanical and dielectric properties. PEEK has good chemical resistance. However, a potential clinical disadvantage of intervertebral disc implants, is that PEEK alone is not bioactive. Surface functionalization of medical devices made of polyaryletheretherketone (PEEK) is an essential requirement when a direct osteointegration between implants and host tissues is desired. The main objective of the work was to improve bio- activity and tribological properties of advanced polymer PEEK type materials through development of biomimetic, smart polytetrafluorethylene (PTFE) composite coatings. The optimal biological and tribological properties of the PTFE coating were found for porous, nano- composite, multi- layered structures. Coatings were porous on the surface, which was prone for fibroblast cell proliferation, and more dense close to the PEEK substrate, what positively influenced on their tribological properties. Acknowledgment: This work was supported by the National Science Centre (Narodowe Centrum Nauki, abbr. NCN) No: 2014/15/B/ST8/00103

Authors : Bum Ho Choi, Moon Hee Kang, Eun Mi Kim, and Jong Ho Lee
Affiliations : Center for Nano-Photonics Convergence Technology, Korea Institute of Industrial Technology

Resume : In this paper, we describe a developed and characterized liquid precursor delivery system (LDS) for preparation of a water-vapor permeation-barrier layer in organic electronic devices. The proposed LDS consists of three major parts: 1) an aerosol generator that transforms the liquid precursor into an aerosol molecule by a piezoelectric ultrasonic vibrator, 2) a vaporizer that transforms injected aerosol molecules into a vapor state, and 3) vapor storage canister. The instant evaporation fraction and maximum evaporation mass rate were measured to be 98.3% and 2.55 g/min, respectively. The temperature in the vaporizer was very stable, showing only 1oC of a difference from the set temperature. As the temperature in LDS increased, the evaporation mass rate increased from 0.035 to 2.55 g/min. A 30-nm-thick SiN layer was prepared to evaluate the performance of LDS, which was attached to a cyclic-chemical vapor deposition system. The prepared SiN layer exhibited a very smooth surface with no defects and pinholes. The roughness of the prepared SiN film was measured to be 1.25 nm in the root mean square value, which is comparable to conventional bubbler type LDS. The water vapor transmission rate obtained from the 30-nm-thick SiN layer was measured to be 1.31×10-6g/m2/day. That measurement meets the requirement for organic electronic device applications, such as organic thin-film transistors, organic solar cells, and organic light-emitting diodes.

Authors : Heetak Han, Jungmok Seo,Sera Shin, Hyunchul Kim, Taeyoon Lee
Affiliations : Nanobio Device Laboratory, School of Electrical and Electronic Engineering, Yonsei University

Resume : Droplet-based microfluidic systems have received broad attentions since they allow sufficient chemical and biological analyses with only small amount of specimen and reagents. Compared to the continuous flow-based microfluidics, which need complicated channel networks, droplet-based microfluidic systems can supply more versatility. Recently, novel droplet-based microfluidics have been developed using superhydrophobic surface, enabling the droplet manipulation without any additives. However, despite its advantage, it still has limitation to manipulate the low-surface tension liquid, which prohibits the application of diverse bioassay. Herein, we developed the new class of droplet manipulation platform using flexible superomniphobic substrate and local vacuum suction device. Flexible superomniphobic substrate was made by spray coating of fluorinated SiO2 nanoparticle. When the negative pressure was applied below the substrate by using the vacuum tip, local dimple was generated. Since adhesion force between the substrate and the droplet there was very small, the droplet can be guided in the local dimple by the gravitational force. In addition, we demonstrated a few micro-litter droplet patterning technique using fabricated system with partial superhydrophilic patterning. Based on the system, we could precisely analyze the concentration of glucose in a sample droplet. This platform may give a chance to proceed the bioassay area and may be used in diverse experiments such as chemical synthesis and colorimetric multiplex bioassay.

Authors : Shabnam Karimi(a,b), Fatemeh Mahzoon(a), Kamal Janghorban(a), Siroos Javadpour(a)
Affiliations : a) Shiraz University, Department of Materials Science and Engineering b) Austrian Institute of Technology, Department of Biosensors Technology

Resume : The aim of this study is to provide HA-ZrO2 ceramic coatings on 316L stainless steel and titanium by cathodic plasma electrolytic deposition technique and to investigate it’s biocompatibility in artificial saliva and Ringer’s solution. The process was performed in K2ZrF6 electrolyte solution. The surface layer chemical compositions were analyzed by X-ray diffraction (XRD) and it was shown the formation HA-ZrO2 on the substrates. Scanning electron microscope (SEM) was used to observe the unique morphology of the surface layers. The corrosion resistance of the coated surface was investigated by electrochemical studies involving cyclic voltammetery method in artificial saliva and Ringer’s solution. The results showed a corrosion resistance improvement due to the variation in composition and unique surface morphology. Wear resistance and friction coefficient were investigated using pin on disc wear test. The unique morphology of the surface layer caused the improvement of wear resistance and friction coefficient. Also Roughness and hardness of the samples were measured. The results indicated the significant increasing effect of PED treatment on the surface roughness and hardness. With analogy between the results, it can be concluded that HA-ZrO2 coated 316L stainless steels are good substitutes for titanium in implantology for manufacturing osseointegrated implants like hip and knee replacement, shoulder and elbow joints replacement and also dental implants.

Authors : S.I. Eguía-Eguía*, O. Fuentes-Ramírez*, J. Santoyo-Salazar**, J.R. Aguilar-Hernández***, P. Maldonado-Altamirano***, L. Gildo-Ortiz*
Affiliations : *Doctorado en Nanociencias y Nanotecnología, Centro de Investigación y de Estudios Avanzados del Instituto Politécnico Nacional, CINVESTAV-IPN, Av. IPN 2508, Zacatenco, 07360, Mexico **Departamento de Física, Centro de Investigación y de Estudios Avanzados del Instituto Politécnico Nacional, CINVESTAV-IPN, Av. IPN 2508, Zacatenco, 07360, Mexico ***Instituto Politécnico Nacional, Av. Luis Enrique Erro S/N, Zacatenco, 07738, México

Resume : Nowdays, the development of functionalized nanoparticles has an important growth, because of their future possibilities and applications in cancer treatment. Functionalized magnetite nanoparticles can be used as magnetic domains core with an organic bicompatible shell to add complex systems. In this work, magnetite nanoparticles have been synthesized with different batches, via co-precipitation at 80°C from ferrous Fe(2) and ferric Fe(3) ions, under an inert atmosphere. In one of the batches, during the synthesis, 3-amino-1-propanol was used as a reducing agent and stabilizer. In the other synthesis, the magnetite nanoparticles were aminated through silanization, using 3-aminopropyltriethoxysilane (APTES), as linker. The amine-magnetite nanoparticles enable the covalent conjugation of a paramagnetic gadolinium complex Gd- diethylenetriaminepentaacetic acid (DTPA). The surface of these nanoparticles was functionalized with (DTPA) via carbodiimide chemistry; where the DTPA acts as complexing agent for the introduction of gadolinioum ions on the surface of the nanomaterial. Morphology, particle size, structure and magnetic properties of the as-prepared nanocomposites were charcaterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman Spectroscopy, Transmission Electron Microscopy (TEM), Vibrating Sample Magnetometer (VSM), Fhotoluminiscence and Magnetic Force Microscopy (MFM) to define their physical properties as contrast agents.

Authors : Brigita Abakevičienė(1,2), Dalius Jucius(1), Viktoras Grigaliūnas(1), Algirdas Lazauskas(1), Saulius Smetona(3), Sigitas Tamulevičius(1)
Affiliations : (1) Institute of Materials Science, Kaunas University of Technology, Barsausko str. 59, LT-51423 Kaunas, Lithuania (2) Department of Physics, Kaunas University of Technology, Studentu str. 50, LT-51368 Kaunas, Lithuania (3) Qorvo, 7628 Thorndike Road Greensboro, NC 27409 United States

Resume : Fluoropolymers are increasingly used for the mass production of microoptical elements as they are sufficiently stable, reliable, UV transparent materials and can replace the expensive quartz, for example, producing microlenses. In this study, UV nanoimprint lithography using rigid polymer molds was succesfully applied for the patterning of microlenses in OrmoComp polymer layer drop-deposited on the ETFE and FEP fluoropolymers substrate. Adhesion of ETFE and FEP fluoropolymers surface was significantly improved using H2 plasma treatment for 1-3 min at RF source power density of 0,5 W/cm2 under operating pressure of 1.3 Pa and hydrogen flow rate of 100 standard cubic centimeters per minute (sccm). The surface energy of H2 plasma treated ETFE and FEP fluoropolymers increased substantially, thus significantly enhancing the wettability and adhesion properties. Aging tests show, that H2 plasma treatment of fluoropolymer films have long-term effect and does not cause any defects, affecting behaviour of microlenses.

Authors : M. Dinu (1), T. Hauffman (2), A. Vladescu (1), A. Hubin (2), M. Braic (1)
Affiliations : (1) National Institute for Optoelectronics (INOE 2000), 409 Atomistilor St., Magurele, Romania; (2) Vrije Universiteit Brussel, Department of Materials and Chemistry, Research Group Electrochemical and Surface Engineering, Pleinlaan 2, 1050 Brussels, Belgium

Resume : Dental frameworks made of ceramic veneered CoCr alloy are widely used in dentistry due to their superior mechanical properties and favourable aesthetics. However, their clinical performance is affected by the biological environment leading to partial removement of the ceramic layer, leaving larger areas of metal exposed to the aggressive oral environment. We report on three multilayers (CrSiN/CrSiON, CrSi/CrSiN/CrSiON and Cr/CrSi/CrSiN/CrSiON) obtained by cathodic arc method and used to overcome the failure of dental prosthesis by improving the bond strength between CoCr framework and ceramic component. An overview on the behaviour of the coated CoCr alloy was carried out by in vitro studies in simulated body fluids, from both corrosion and biocompatibility points of view. The results indicated that the protection efficiency increases with the number of interfaces, blocking the penetration of the electrolyte through the pores of the coating. Cell viability was found to be high for all the coated samples. During 3-points bending tests the coated Cr/CrSi/CrSiN/CrSiON substrates of CoCr covered with dental ceramic exhibited the best behaviour, associated with the coatings' highest surface roughness and hydrophilicity. This finding can be related to the presence of Cr layer at the CoCr interface, which provided a better adhesion by superior chemical affinity. We acknowledge the support of the Romanian Research and Innovation Ministry, projects PN, PN

Authors : Koo-Hyun Chung, Khac Bien Cuong Tran
Affiliations : School of Mechanical Engineering, University of Ulsan, Ulsan 680-749, Republic of Korea

Resume : Atomically thin molybdenum disulfide (MoS2) has attracted extensive attention because of its remarkable mechanical and electronic properties, and low friction characteristics. Raman spectroscopy has been widely used to characterize the thickness and the thickness-dependent material properties of atomically thin MoS2 owing to the sensitivity of the vibrational spectrum to the thickness. However, the focused laser may increase the surface temperature, which in turn results in surface damage on the upper layers of the MoS2. This laser-induced thermal effect can further influence the aforementioned material properties. In this work, the effects of laser on surface of atomically thin MoS2 were systematically investigated using atomic force microscopy (AFM) and Raman spectroscopy. Single and a few layers MoS2 flakes were prepared by mechanical exfoliation and they were treated by lasers with various powers. AFM topography and friction force images were obtained before and after laser treatment. The result showed that particles were formed on the top surface of MoS2 due to the laser-induced thermal effect. It was also found that degree of the particle formation was dependent on the laser power and the thickness of MoS2. Furthermore, the particle formed on MoS2 surface caused the significant increase in friction force. The outcomes of this work may be useful for the thermal management in the design of nano-devices based on atomically thin MoS2.

Authors : Marta Tessarolo 1-2, Elisabetta Rotante 1, Nicole Ticchi 1, Filippo Capelli 1, Beatrice Fraboni 2, Maurizio Fiorini 3, Vincenza Andrisano 4, Vittorio Colombo 5, Santina Romani 6
Affiliations : 1 Interdepartmental Centre for Industrial Research – Advanced Mechanics and Materials (CIRI – MAM); 2 Department of Physics and Astronomy, University of Bologna, Bologna, Italy ; 3 Department of Civil, Chemical, Environmental, and Materials Engineering University of Bologna, Bologna, Italy; 4 Department for Life Quality Studies University of Bologna, Bologna, Italy; 5 Department of Industrial Engineering University of Bologna, Bologna, Italy; 6 Dipartimento di Scienze e Tecnologie AgroAlimentari University of Bologna, Bologna, Italy;

Resume : The development of new bio-compostable materials has attracted much attention in the field of food packaging. However, the main drawback of biodegradable films is the low barrier they offer against external agents that can quickly degrade foods, limiting their use to a small number of products. To overcome this issue, we developed a new active multilayer film, bio-compostable with excellent oxygen scavenging proprieties, able to increase the shelf-life of food products obtained without the use of preservative agents. The oxygen scavenging activity is obtained by including in the multilayer film system a layer of glucose and glucosidases that catalyzes the oxygen absorption. Both molecules and enzyme are dissolved in a polymer matrix based on PVOH and deposited on a PLA film, following an appropriate treatment with plasma to increase the hydrophilicity, allowing a uniform coating. The plasma treatment is performed in air with an in-line reactor chamber included in the film-forming machine. The main effect is to increase the number of alcohol and methyl groups, enhancing the contact angle and guaranteeing a perfect coating with the active gel solution. In order to monitor the efficiency of the innovative active packaging a sensor based on a conductive polymer has been developed, that, used as an ink, is stamped on the PLA surfaces after the plasma treatment. The final PLA multilayer film with high oxygen scavenging activity, being totally biodegradable, can perfectly implement a “green” food packaging.

Authors : Márton Szendrő, Péter Süle
Affiliations : Hungarian Academy of Sciences, Centre for Energy Research, Institute for Technical Physics and Materials Science, Konkoly-Thege Miklós u. 29-33, Budapest, Hungary

Resume : One problematic aspect of graphene (GR) CVD growth on metal substrates is that GR is capable to create rotational domains [1], separated by grain boundaries (GBs), sometimes even on a single crystal surface [2]. GBs worsen the electric properties of GR[3], therefore the nucleation of differently orientated islands is an undesirable phenomenon. An interesting feature is, that the different existing orientations are very specific to the substrate (e.g: on Cu(111) the most commonly known orientations are: R0°, R7°, but for Ir(111) we have R0°, R14°, R19°, R23°, R26°, R30°)[4]. Even today there is no such a physical model that can somehow clarify the very basic nature of these orientations. Why only these orientations can appear, and what are the circumstances that influences the GR to realize one or another? In order to understand these aspects we developed a continuum mathematical model that calculates the adhesion energy of a GR island with a given size and orientation only by knowing the underlying Moiré-pattern that is formed between the atomic lattices. Our model agrees surprisingly well with DFT and CMD results. This shows that we have captured some very basic physical insights of the adhesion. Using our model Monte-Carlo (MC) simulations can be carried out to perform GR growth simulations on several germs to analyze their distribution of orientation. These MC simulations are several orders of magnitude faster than Kinetic MC methods. References: [1] M. Batzill, Surf. Sci. Rep. 67, 83 (2012). [2] Li Gao, Jeffrey R. Guest, Nathan P. Guisinger, Nano Letters 10(9), 3512-3516. (2010). [3] Vancsó, Péter, et al., Applied Surface Science 291, 58-63 (2014). [4] Tetlow, H., et al., Physics Reports 542.3, 195-295 (2014).

Authors : Stephen M. Ubnoske (1), Erich J. Radauscher (2), Eric R. Meshot (3), Brian R. Stoner (4), Charles B. Parker (2), and Jeffrey T. Glass (2)
Affiliations : (1): Department of Mechanical Engineering and Materials Science, Duke University, Durham, NC 27708, USA (2): Department of Electrical and Computer Engineering, Duke University, Durham, NC 27708, USA (3): Physical and Life Sciences Directorate, Lawrence Livermore National Laboratory, Livermore, CA 94551, USA (4): Research Triangle Institute (RTI) International, Durham, NC 27709, USA

Resume : The growth of carbon nanotubes (CNTs) on polycrystalline silicon substrates was studied to improve the design of CNT field emission sources for microelectromechanical systems (MEMS) applications and vacuum microelectronic devices (VMDs). Microwave plasma-enhanced chemical vapor deposition (PECVD) was used for CNT growth, resulting in CNTs that incorporate the catalyst particle at their base. The kinetics of CNT growth on polysilicon were compared to growth on Si (100) using the model of Deal and Grove, finding activation energies of 1.61 and 1.54 eV for the nucleation phase of growth and 1.90 and 3.69 eV for the diffusion-limited phase on Si (100) and polysilicon, respectively. Diffusivity values for growth on polysilicon were notably lower than the corresponding values on Si (100) and the growth process became diffusion-limited earlier. Evidence favors a surface diffusion growth mechanism involving diffusion of carbon precursor species along the length of the CNT forest to the catalyst at the base. Explanations for the differences in activation energies and diffusivities were elucidated by SEM analysis of the catalyst nanoparticle arrays and through wide-angle X-ray scattering (WAXS) of CNT forests. Finally, methods are presented to improve adhesion of CNT films during operation as field emitters, resulting in a 2.5x improvement.

Authors : Kudryashov Dmitry, Monastyrenko Anatoly, Gudovskikh Alexander
Affiliations : St. Petersburg National Research Academic University RAS

Resume : Semiconductor heterostructures are widely used in device fabrication. A lot of modern transistors, lasers and solar cells are manufactured using heterojunctions. Portable optoelectronic gas sensors operating in the IR spectral range are already replacing conventional electrochemical monitors. In general the gas is pumped into the chamber and gas concentration is measured electro-optically by its absorption of a specific wavelength. Such sensors can be used to determine a lot of gases including chlorine. It is an important component in the manufacture of conventional materials. At the same time chlorine is a toxic gas that attacks the respiratory system, eyes, and skin. Thus it is very important to measure chlorine concentration in air and aqua solutions. It is known that chlorine gas and its oxygen compounds in solution absorb light in the wavelength range of 300-420 nm [1]. ZnO based photodetectors have a similar spectral range [2]. The combination of UV LED with a ZnO based photodiode can be used in low-cost chlorine sensor. This paper presents some results obtained from an investigation of growth parameters on EQE spectra of ITO/ZnO/Cu2O heterostructure made by magnetron sputtering. A sensitive and low-cost free chlorine sensor has been developed and sensing tests were performed. The reported study was supported by RFBR project №15-08-06645a. [1] Rafaela T.P. et al. // J. Braz. Chem. Soc., 2012. V.23, P.1543-1550 [2] K. Liu et al. // Sensors (Basel). 2010; 10(9): P.8604–8634

Authors : P.V. Borisyuk, Yu.Yu. Lebedinskii, O.S. Vasilyev, T.I. Kozlova, V.V. Fetisov
Affiliations : National Research Nuclear University MEPhI (Moscow Engineering Physics Institute)

Resume : Studies of thin nanocluster films of Mo, Ag, Ta are of great interest due to their possible applications as highly efficient thermoelectric materials. In this work thin nanocluster films of Mo, Ag and Ta were formed on SiO2/Si(001) surface at room temperature using nanocluster source Nanogen-50 with quadrupole mass-spectrometer MesoQ (Mantis Deposition, UK) incorporated into the UHV surface analysis system Multiprobe MXPS VT AFM (Omicron NanoTechnology GmbH, Germany). The chemical composition of thin nanocluster films was controlled in situ by means of X-ray photoelectron spectroscopy. Susceptibility of the films to oxidation was studied ex situ at room temperature and after heating up to 900 K. The size and shape of the clusters in films were measured ex situ by analyzing images obtained with the scanning electron microscope. The band gap value for Ta, Mo films were measured using reflection electron energy loss spectroscopy. Variation of the work function of the films with size of clusters in film were studied. Electronic and chemical properties of films obtained show the potential of further usage of nanocluster films as thermoelectric materials.

Authors : P.V. Borisyuk, Yu.Yu. Lebedinskii, O.S. Vasilyev, Tkalya E.V.
Affiliations : National Research Nuclear University MEPhI (Moscow Engineering Physics Institute)

Resume : Results of experimental studies of thorium ions implantation into thin silicon oxide layers within pulse plasma fluxes expansion are presented. Formation of plasma plumes were initiated in solid-state thorium target in strong electrical fields by nanosecond laser pulses with power density of about several GW/cm2. Depth distribution of thorium atoms in the subsurface area of 10 nm thickness, chemical state of implanted thorium atoms and bandgap of modified silicon oxide film at different conditions of implantation processes were studied with XPS and REELS methods. The results of chemical composition analysis of the surface with XPS and REELS methods show that the compounds obtained in modified silicon oxide film are based on a complex thorium silicates and have bandgap within a range of 6.0-9.0 eV depending on local concentration of thorium atoms. A quantitative assessment of the yield of isomeric nuclei in a “hot” laser plasma at the early stages of expansion was made. The estimations made again with experimental results show that the laser ion implantation of thorium ions in SiO2 matrix can be useful for further research of «nuclear clocks» based on low-lying isomeric transition in 229Th isotope with energy 7.8 ± 0.5 eV.


Resume : Superconductor ferromagnet hybrid structures, which shows different, coupling mechanisms in the interface, have promising applications in spintronics. Generation of spin triplet cooper pairs and longer spin relaxation time in superconductors enables efficient spin injection and dissipation less spin transport. Bi and tri layers of FM/SC/FM structures showed exchange couplings and giant magneto resistance (MR) below their Tc. CoFeB/MgO/CoFeB based magnetic tunnel junctions with its interfacial epitaxy and formation of crystalline interface showed record TMR at room temperatures. Exploiting this interfacial quality, which is responsible for high spin filtering can be used for fabricating CoFeB/MgB2 based hybrid layers. MgB2 superconductor with industrially acceptable critical current density is an excellent choice because of its oriented growth over MgO substrates. We have fabricated CoFeB (100nm)/MgB2 (50nm) hybrid structure through DC sputtering and pulsed laser deposition respectively. This structure has been annealed at 573K to achieve epitaxial formation at CoFeB/MgB2 interface. XRD and XRR measurements showed oriented formation of MgB2 formation over CoFeB and respective thicknesses. Magnetic measurements were done to extract Jc values from Beans extended critical state model. We will discuss in detail about the magnetic properties of CoFeB/MgB2 hybrid structure, which will enable us to fabricate CoFeB/MgB2/CoFeB structure for spin injection and MR studies

Authors : Taewoo EOM, Sang Hyeop Lee, Chan Moon Song, Sang Yong Park, Donggun Lim*
Affiliations : Department of IT convergence, Korea National University of Transportation

Resume : In this study, zinc sulfide(ZnS) thin films were fabricated using a wet chemical process. ZnS thin films were analyzed according to the addition of a complexing agent, the characteristics of ZnS thin films were analyzed by adding EDTA(ethylenediamine tetra-acetate acid), HMTA(hexamethylene tetramine). The morphological characteristics of the ZnS buffer layer are closely related to the use of a complexing agent that controls the concentration of Zn2+ ions in the deposition process. The addition of the complexing agent EDTA accelerated the cluster - cluster method, resulting in faster deposition but lower uniformity and greater cracking phenomenon. HMTA can be effectively applied to increase the amount of Zn2+ ions forming ZnS. it is easily found as Zn2HMTA at high temperatures. The results of the experiment with the addition of HMTA revealed that as the HMTA concentration increased, the surface of the thin film did not change, but the thickness of the thin film increased gradually. HMTA promoted the ion-ion method to grow the thin film uniformly, but the speed was slow. Additionally, experiment with mixed complexing agent was executed. The best ZnS thin film with transmittance of 80.7%, denser surface was prepared by mixing and adding EDTA and HMTA at an HMTA concentration of 0.2 M. However, as the concentration increased, the growth rate of the thin film increased. However, the surface cracked too much to be used as a buffer layer.

Authors : D. Stathokostopoulos, D. Chaliampalias, N. Pliatsikas, S. Kassavetis, E. Pavlidou, P. Patsalas, S. Logothetidis, K. Chrissafis, G. Vourlias
Affiliations : Department of Physics, Aristotle University of Thessaloniki

Resume : Many efforts have been made to improve the surface properties of copper, a material with many applications such as electrical wires and industrial machinery and alternators which are based on copper thermal and electrical conductivity, its malleability and ductility. However, the main disadvantage of copper is its poor oxidation resistance especially at elevated temperatures. The scope of this work is the comparative study of Mg, Al and TiN coatings deposited on commercial copper for the improvement of the surface resistance when exposed in harsh environment. In every case the deposition was accomplished by pack cementation which is a promising low cost and environmental friendly method. It is a thermochemical process which combines a chemical vapor reaction and the solid state diffusion step. The experiments were undertaken at temperatures from 500 to 600ο C for Mg and Al and from 850 to 1000ο C for TiN coatings, while the holding time was 2h in every case. The structure of the coatings was examined with X-Ray diffraction, X-ray photoelectron spectroscopy and electron microscopy. Selective specimens were examined for oxidation resistance by thermogravimetric analysis and for surface hardness by nanoidentation. It was revealed that in every case thick uniform coatings were formed which were found to offer improved oxidation resistance under high temperature air exposure. Finally TiN coatings were revealed to increase the surface hardness of the Cu coupons.

Authors : Florian Bartoli, Philippe Pigeat, Thierry Aubert, Omar Elmazria, Pascal Boulet, Jaafar Ghanbaja.
Affiliations : Florian Bartoli(1,2); Philippe Pigeat(2); Thierry Aubert(1,3); Omar Elmazria(2); Pascal Boulet(2); Jaafar Ghanbaja(2). 1. CentraleSupélec, Laboratoire LMOPS, Metz, France 2. Institut Jean Lamour, UMR 7198 CNRS-Université de Lorraine, Vandoeuvre-lès-Nancy, France 3. Laboratoire SYMME, Université Savoie Mont Blanc, Annecy-le-Vieux, France

Resume : Surface acoustic waves (SAW) devices are key components in communication systems. They are also intensively studied as wireless sensors, especially since they have demonstrated good operability in harsh conditions. Because of their unique combination of high acoustic velocity, large electromechanical coupling and good stability in harsh conditions, ScxAl1-xN thin films are highly valuable for various SAW applications. The aim of this work is to achieve highly-textured c-oriented ScxAl1-xN thin films, with a FWHM rocking-curve below 1° to maximize the piezoelectric properties of the film, for various Sc rates (0 ≤ x ≤ 0.4). The films are deposited by reactive magnetron sputtering on sapphire substrates, with a composite target. The microstructure is determined by θ-2θ, rocking-curve and pole figure X-ray diffraction (XRD) measurements. Transmission electron microscopy is used to observe the nanostructure, and the atomic ratio is measured by Energy dispersive X-ray spectroscopy. Firstly, AlN thin films with a strong (002) orientation (mosaicity < 0.5°) were deposited to get a reference sample without Sc. Then, the deposition parameters were adjusted to grow highly-textured c-oriented Sc0.07Al0.93N and Sc0.14Al0.86N films. XRD measurements show a strong (002) orientation for both compositions with a mosaicity below 0.9°. TEM micrographs show epitaxial growths at the substrate interface. Ongoing experiments are dedicated to the optimization of the film texture for higher Sc rates.

Authors : S.I. Sidorenko1, Ie.V. Ivashchenko1, G.G.Lobachоva1, V.I. Panarin2, O.M. Hubina1, V.V. Yanchuk1
Affiliations : 1 Metal Physics Department, Igor Sikorsky Kyiv Polytechnic Institute, Ukraine; 2 G. V. Kurdyumov Institute for Metal Physics of the National Academy of Science of Ukraine.

Resume : The feature of coatings for bone and dental implants is the ability to link with living bone. There is appropriate strengthening of coatings, using carbon nanotubes (CNT), which also show high rates of biocompatibility, and final laser surface treatment of finished implant to obtain such properties as strength, surface finely porous and corrosion resistant layers. The CNT were grown on a substrate of silicon oxide using the modified method of Cathodic Arc Evaporation. There was used a metal catalyst (Fe) to fix the carbon nanotubes on the substrate surface. Diameter of nanotubes on the surface of SiO2 is 15 - 25 nm. There were used such binders as glycerin, polyethylene glycol (PEG) and Vaseline to consolidate hydroxyapatite on the surface of the plate. These compounds are organic. There are carbon and hydrogen, elements that form the basis of biological fluids and tissues, in their chemical composition. There was done trial laser alloying to determine which of the agents is the best for this type of treatment. The best results shoved Vaseline. In this environment hydroxyapatite melted well and was uniformly covered on the substrate surface. There was held laser alloying of the surface with different energies (from 1 J to 5 J) of laser beam to get the desired properties of the coating and to prevent the overheating of the surface material. In the case of the laser beam with the energy E = 1 J hydroxyapatite melts well and evenly covers the surface of the base material. The thickness of hydroxyapatite layer was 100 microns.

Authors : Yen-Chang Chiang 1, Shun-Huei Wang 1, Guan-Ting Hou 1, Jeng-Ting Li 1, Jiann-Shing Jeng 2, Jen-Sue Chen 1
Affiliations : 1 Department of materials science and engineering, National Cheng Kung University, Tainan 70101, Taiwan; 2 Department of Materials Science, National Tainan University, Tainan 70005, Taiwan

Resume : Attributed to their high mobility and low temperature process, amorphous metal oxides have replaced silicon as main semiconductor materials in the thin-film transistors (TFTs). In AOS (amorphous oxide semiconductor) TFTs, the existence of sub-gap states plays an important role in electrical performance. In previous studies, the density of acceptor-like states (gA(E)) could be extracted from multi-frequency C-V and density of donor-like states (gD(E)), in other hands, is obtained by fitting I-V curves. In this study, we will get both gA(E) and gD(E) simultaneously, based on optical response of C-V characteristics of TFT. The C-V data of AOS TFT obtained under dark and light (532 nm) illumination are modeled separately in two gate voltage regions. For the gate voltage larger than flat band voltage, the TFT device acts as two capacitors in series (capacitance of active layer and dielectric layer) and the capacitors are extending from source to drain. However, for gate voltage smaller than flat band voltage, the capacitors are formed only for the area right under source/drain electrodes. With these two different models, gA(E) and gD(E) can be acquired; therefore, the energy-dependent sub-gap state profile is obtained simply by fabricating a TFT device.

Authors : A. Etiemble 1, G. Nkou Bouala 2, C. Der Loughian 2, P. Steyer2, J.F. Pierson1
Affiliations : 1 Institut Jean Lamour (UMR CNRS 7198), Université de Lorraine, Parc de Saurupt, 54011 Nancy, France 2Univ. Lyon, INSA-Lyon, MATEISUMR CNRS 5510, 21 Avenue Jean Capelle, 69621, Villeurbanne cedex, France

Resume : Thin film metallic glasses (TFMG) has recently emerged as alternative materials for many applications, such as micro-electro-mechanical systems, micro- or nano-replication and biomedical use [1,2]. Physical vapor deposition (PVD) techniques like magnetron sputtering make possible synthesis of TFMG in an extended range of compositions. It has for example been demonstrated that binary Zr-Cu films [13-85 at.%Cu], presenting a glassy-like microstructure, can be obtained using pure Cu and Zr targets [3]. In this study, we focused on the ability to form TFMG from binary Zr-Ag, binary Zr-Cu and ternary Zr-Cu-Ag systems using PVD magnetron co-sputtering processes. Both static and rotating substrate holder configurations were performed for the three systems. The chemical composition of the films was obtained by energy dispersive X-ray spectroscopy, the structure was characterized by X-ray diffraction and the microstructure by scanning electron microscopy. In the static configuration, the composition of the films can be associated with the substrate position relative to the targets, while it can be controlled by the current applied to the targets in the rotating configuration. The influence of process configuration and composition on the structure and microstructure of the thin film was investigated. [1] J.P. Chu et al., Thin Solid Films 520 (2012) 509-5122 [2] A. Etiemble et al., J. Alloys and Comp. (2016) [3] M. Apreutesei et al., Thin Solid Films 561 (2014) 53-59

Authors : Diana Maria Vranceanu1, Mihaela Dinu2, Funda Ak Azem3, Radwan Abdulgader4, Viorel Braic2, Isil Birlik3, Adrian Kiss2, Cosmin Mihai Cotrut1, Robyn Booysen5, Mariana Braic2, Thomas K. Monsees4, Alina Vladescu2
Affiliations : 1University Politehnica of Bucharest, 313 Spl. Independentei, Bucharest, Romania; 2National Institute for Optoelectronics, 409 Atomistilor St., Magurele, Romania; 3 Dokuz Eylul University, Engineering Faculty, Metallurgical and Materials Engineering Department, Tinaztepe Campus, Izmir, Turkey; 4Department of Medical Biosciences, University of the Western Cape, Bellville, South Africa

Resume : Hydroxyapatite (HAP) coatings are applied on Ti6Al4V metallic substrate to combine mechanical property of Ti6Al4V alloy with bioactivity property of HAP. In this study, HAP coatings with additions of SiC and Mg are proposed to be deposited on Ti6Al4V substrates by RF magnetron sputtering technique in order to improve the mechanical properties and to decrease the dissolution rate in simulated body fluid (SBF) of undoped HAP. Chemical bonding, morphology, mechanical and biological properties, corrosion resistance and degradation rate in SBF at 37 °C of the coated surfaces were evaluated. It was found that the SiC and Mg addition does not influence the formation of a stoichiometric structure of the HAP. All coatings exhibited smooth surface and uniform growth, without defects or cracks. The elastic modulus of doped coatings has a value more closely to those of human bones. The doped HAP coatings were found to enhance the corrosion resistance of the Ti6Al4V alloy in the SBF solution. The best corrosion resistance was found for the coatings with a smooth surface. A significant decrease of the mass loss rate of the Ti6Al4V alloy after coatings was found. The doped coatings have low degradation rate compared to uncoated substrate and undoped HAP. All of the investigated coatings were biocompatible as demonstrated by SaOS-2 bone cells attachment and growth. However, proliferation and morphology of cells grown on the coatings was somehow inferior than on uncoated Ti6Al4V.

Authors : M. Danek, F. Fernandes, A. Cavaleiro, T. Polcar
Affiliations : Department of Control Engineering, Faculty of Electrical Engineering, Czech Technical University in Prague, Czech Republic; SEG-CEMUC, Department of Mechanical Engineering, University of Coimbra, Rua Luís Reis Santos, 3030-788 Coimbra, Portugal;; SEG-CEMUC, Department of Mechanical Engineering, University of Coimbra, Rua Luís Reis Santos, 3030-788 Coimbra, Portugal; nCATS, Highfield Campus, University of Southampton, Southampton SO17 1BJ United Kingdom

Resume : Ti1?xAlxN coatings with NaCl-type structure have been widely used in advanced machining and other high temperature applications due to their excellent mechanical, thermal and tribological properties. Here, we investigated the influence of Cr additions on the structure, mechanical properties and oxidation resistance, including the oxide scale characterization, of multilayered TiAlN/CrAlN coatings deposited by magnetron sputtering. The properties of Cr rich coatings were compared to a TiAlN film deposited as reference. XRD diffraction analysis revealed that all coatings showed an fcc NaCl-type structure. However, for the TiAlN monolayer Ti and Al are forming a solid solution whilst, for Cr rich coatings, a multilayer structure alternating TiAlN and CrAlN layers, also forming solid *Manuscript Click here to view linked References solutions, was grown as a result of the geometry of the targets distribution inside the deposition chamber in combination with a slow rotation of the sample holder and a sufficiently high deposition rate. TGA measurements showed that Cr additions increased the oxidation performance of the coatings. For Ti0.47Al0.46N, dual oxide layers occur when tested at 800 ºC, being the porous inner one of TiO2 and the outer a compact and continuous layer of Al-oxide which protects the coating from the oxidation. At 900 ºC the oxidation resistance of this film degraded due to the fast Ti ions diffusion to the surface which impedes the formation of the continuous and protective Al oxide layer. Cr rich coatings showed different oxides scales depending on their chemical composition. For Ti0.30Al0.46Cr0.26N and Ti0.28Al0.34Cr0.42N, a Ti-O rich layer is formed on the top of a protective Al-Cr-O layer when the samples were tested at 900 ºC and 1000 ºC, being the oxide layers thicker for the higher temperature. Concerning the coating with the highest Cr content (Ti0.28Al0.31Cr0.51N), a compact and continuous Cr(Al)2O3 oxide layer was formed at 900 and 1000 ºC with residual TiO2 islands on the top, contributing for a significant enhancement of the oxidation resistance.

Authors : Sisir Chowdhury, Pallab Banerji
Affiliations : Indian Institute of Technology Kharagpur

Resume : Though growth of indium gallium arsenide epitaxial layer on indium phosphide substrate is well reported, but for the micro-electronic application with the silicon based process technology, we need to transfer it to the Si substrate for monolithic integration circuits to fabricate high speed device. Moreover, Silicon substrate is less expensive and available with larger diameter than any other wafers. As, direct epitaxial layer growth of InGaAs is on Si substrate could not be achieved, other than low dimensional structures, a buffer layer of InP on Si can be introduced to get a lattice matched substrate. In our present investigation we tried to deposit InxGa1-xAs layer by Metal Organic Chemical Vapor Deposition (MOCVD) technique on Si substrate followed by an InP buffer layer. Indium gallium arsenide layer with indium phosphide buffer has been grown on p-type silicon (100) by Metal Organic Chemical Vapor Deposition (MOCVD) technique. The composition and the crystalline quality of the grown films have been investigated by UV-Vis-NIR reflectance spectroscopy and grazing incidence X-ray diffractometry (GIXRD). To get a lattice matched substrate an InP buffer layer is deposited onto Si substrate prior to InGaAs growth. The reflectance spectrum shows the band gap energy of the grown InGaAs layers are determined to be 0.82 eV and from the diffraction data the lattice constants of the grown layers are found to be 5.855 and 5.875 nm for two growth temperatures of 6000C and 650 0C for same precursors flow rates. Applying Vegard?s law, it is found that the results found from these two different techniques are consistent. The thickness and the growth rate are determined from the reflectance spectrum. It is found that the deposition lies in the mass transport limited regime for the mentioned temperature range.

Authors : C. Furgeaud, A. Michel, C. Mastail, L. Simonot, G. Adadias
Affiliations : Institut Pprime, UPR 3346, Université de Poitiers-CNRS-ENSMA, France

Resume : Polycrystalline metallic films growing in a Volmer-Weber mode, as typically encountered during condensation of metal vapors on insulating substrates, are technologically important in a variety of applications, such as catalysis or plasmonics for which nanoparticle synthesis is a requisite. The nucleation, coalescence and continuous film growth stages of high-mobility metals are associated with a compressive-tensile-compressive behavior, as evidenced using real-time stress diagnostic. As the lateral grain size is usually set-in during the coalescence stage, controlling the nucleation conditions is of paramount importance for tuning the films properties as well as stress levels. This can be achieved by changing the substrate temperature or deposition flux. Here we employ Ge surfactant to vary the nucleation conditions during sputter-deposition of Cu films, and use a combination of in situ and real-time techniques to monitor the growth. We identify the percolation thickness from electrical resistivity measurements, while the onset of film continuity is determined from the maximum tensile force using a multiple beam optical stress sensor. Complementary analyses using atomic force and transmission electron microscopy are employed to obtain information on the growth morphology and grain size.

Authors : Viktor S. Gurov, Michael V. Dubkov, Sergey M. Karabanov, Dmitry V. Suvorov, Yulia M. Stryuchkova, Gennady P. Gololobov, Dmitry Yu. Tarabrin
Affiliations : Ryazan State Radio Engineering University, Ryazan, Russia

Resume : One of the key problems systems of electron and ion optics (mass spectrometers, ion trap, quadrupole systems, ion and electron transport systems) is a distortion of the electric field within the electrode system. The main cause of the distortion is the formation non-conductive polymeric hydrocarbon films on the electrodes surface, which are charged by the charged particle (ions and electrons) and causes significant distortion of electric field configuration. The traditional way to reduce the rate of formation of the films is continuous heating electrode system to 150-180 ° C, which results in high power consumption and causes additional distortions caused by thermal deformations. The paper presents a method of synthesis and characteristics of multilayered Indium-based functional coating provides effective removal of hydrocarbon-polymer film on electrodes surface. The self-cleaning physical principle consists in electrode system heating (periodic) to a temperature of 110-160 ° C causing melting Indium external layer of coating (about microns thickness). As a result of the melting of the external Indium layer of hydrocarbon-polymer film break and dissolve therein. The paper presents data on the optimal coating structure and thickness, at which the effective retention of the molten coating layer. The multilayer coating comprises an adhesion layer of copper and nickel barrier layer for increasing the number of effective absorption cycles. The paper presents the spatial distribution of elements on the coating thickness profile over time (after a few cycles). It was found that in the process of mutual diffusion of copper and indium. It is shown that the use of the Self-cleaning Indium-based functional coating results in a significant increase in the lifetime of devices electron and ion optics to 4-5 thousand hours. Experimental check has confirmed the advantages of the method of "self-cleaning" surfaces of the electrodes and, as a result, recovery of operating parameters of the mass spectrometer.

Authors : Yu Ra Jeong, Jeonghyun Kim, Sang Min Won, Geumbee Lee, Sang Woo Jin, Soo Yeong Hong, John A. Rogers, Jeong Sook Ha
Affiliations : 1 Department of Chemical and Biological Engineering, Korea University, Seoul, Korea 2 Department of Materials Science and Engineering, Frederick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, Urbana 3 KU-KIST Graduate School of Converging Science and Technology, Korea University, Seoul, Korea

Resume : Skin-like, body attachable devices can be used in a variety of applications ranging from health monitoring systems and human-machine interfaces. They typically demand wireless capabilities to eliminate the physical bulk associated with power sources and obstacles associated with hard-wired connections to external data acquisition systems, respectively. Here, we report on a stretchable human motion monitoring system using GaInSn, a liquid phase eutectic metal alloy, with wireless capabilities using near-field-communication (NFC) technologies. Liquid metal traces were patterned on elastomer substrates via selective surface wetting of reduced GaInSn on a pre-patterned Au films. Complex patterns with resolution of 50 μm were achieved via this process. The liquid metal traces serve as a resistor-type strain sensor, electromagnetic antenna and electrical connections simultaneously in the integrated system. The fabricated strain sensor showed excellent durability for 10,000 stretching cycles under 30% strain, with a gauge factor of 2. Electrical and mechanical analysis of the sensor and inductive coil antenna including excremental measurements and theoretical simulations were performed for various deformations such as tensile (up to 30%) and compressive strains (up to 100 kPa). The demonstrations of motion monitoring include wrist flexion, movements of the vocal cord, and finger motions.

Authors : M.D. Ionita, E.R. Ionita, V. Satulu, B. Mitu, G. Dinescu
Affiliations : National Institute for Laser, Plasma and Radiation Physics Atomistilor 409 Str., 077125 Magurele, Bucharest, Romania

Resume : For reducing the risk of infections, the utilization of antimicrobial surfaces is mandatory. Methods for obtaining such surfaces are thoroughly investigated. Among possible approaches for obtaining antimicrobial surfaces are those based on cold atmospheric pressure plasmas. In this work we report on the deposition of silver-polymer nanocomposites by using an Atmospheric Pressure Discharge with Bare Electrodes (DBE) generated in argon. Ag nanoparticles admixed with HMDSO vapors are introduced in the remote discharge by means of an atomizer system working under continuous oxygen flow, leading to deposition of thin layers of silica-like matrix in which silver is embedded. Composition, chemical bonding and distribution of nanoparticles inside the nanocomposites were corelated to the experimental conditions as regarding the gaseous flows and precursors concentration. Surface morphology, topography and wettability characteristics were investigated in order to determine the optimal parameteres in respect to the desired surface properties. The potential of this method for obtaining highly efficient antibacterial surfaces at low cost is discussed. This work has been financed by the Romanian Ministry of Research and Innovation in the frame of Nucleus programme-contract 4N/2016 and PlasmaTex M-ERA-NET contract 31/2016.

Authors : N. Pliatsikas, G. Vourlias, P. Patsalas
Affiliations : Department of Physics, Aristotle University of Thessaloniki, Thessaloniki, GR-54124, Greece; Department of Physics, Aristotle University of Thessaloniki, Thessaloniki, GR-54124, Greece; Department of Physics, Aristotle University of Thessaloniki, Thessaloniki, GR-54124, Greece

Resume : In this work we have developed plasmonic Ag nanoparticles supported on Si substrates via a simple electroless deposition process eliminating the need of vacuum technology. The near- and far-field plasmonic performance of the produced nanoparticles were evaluated by surface-enhanced Raman scattering (using Rhodamine 6G as test molecule) and specular spectral reflectivity measurements, respectively. The factors influencing the development of nanoparticles, such as the type (p- or n-) and the orientation [100] or [111] of the substrate, the deposition time and the solution’s concentration were studied thoroughly by optical measurements, x-ray diffraction, auger electron spectroscopy and x-ray photoelectron spectroscopy. The deposition time, as well as the concentration, affected significantly the development and the growth rate of the particles making this technique an easy and inexpensive method for the development of tunable plasmonic nanoparticles. The produced plasmonic templates had improved signal-to-noise ratio by an order of magnitude for R6G compared to sputter-deposited Ag nanoparticles

Authors : Hye-Jin Yoo
Affiliations : Surface Technology Research Group., POSCO Technical Research Laboratories 8, Pokposarang-gil, Gwangyang-si, Jeolanam-do, South Korea

Resume : Recently, considerable effort has focused on the functional coating of antibacterial properties in coated steel applications, and which seem to be quite useful in mobile devices, appliances, interior, buildings, and medical stuffs. For this, various bacteria-killing techniques have been developed, such as silver nanoparticles, layer-by-layer (LBL) nanofabrication, incorporation of various antibiotics, and so on. However, the antibacterial coating simultaneously keep up with other requirements like, anticorrosive, high gloss, suitable mechanical properties. In this work, we developed antibacterial coating formulation based on UV steel coating process by using chemically-modified urushiol lacquer. In fact, various kinds of lacquer trees (e.g., toxicodendron vernicifluum) have been used as paints and coating materials for woods and metal surfaces since 5,000 years in oriental culture. This natural lacquer exhibits superior barrier property against oxygen and water, as well as good durability, chemical resistance, and mechanical properties. However, traditional technique based on the enzymatic polymerization needs long time as well as manpower. In addition, pristine urushiol derivatives tend to inhibit free-radical polymerization due to its catechol structure of radical stabilization mechanism. Herein we present a facile method to minimize the radical inhibition for the development of antibacterial, anticorrosive, and high gloss UV coating formulation.

Authors : T.C. Rojas, S. Domínguez-Meister, M. Brizuela, J.C. Sánchez-López
Affiliations : Instituto de Ciencia de Materiales de Sevilla (CSIC- Univ. Sevilla); Instituto de Ciencia de Materiales de Sevilla (CSIC-Univ. Sevilla); TECNALIA, Mikeletegui Pasealekua, 2 20009 Donostia-San Sebastián, Spain; Instituto de Ciencia de Materiales de Sevilla (CSIC-Univ. Sevilla) Avda. Américo Vespucio 49, 41092-Sevilla, Spain;

Resume : CrAlYN hard coatings with two different Al contents (16 and 25 at.%) and Y concentration varying between 1 and 5.7 at. % were deposited by direct current reactive magnetron sputtering on commercial M2 steel substrates by co-sputtering of Cr-Al mixed and Y targets. The samples were heated to 1000 ºC in air during 2 h to study their oxidation resistance and thermal stability. X-ray diffraction, glow-discharge optical emission spectroscopy and transmission electron microscopy coupled with spatially resolved microanalysis techniques were used to investigate the nanostructure, constituent phases and chemical elemental distribution of the as-prepared and oxidized samples. In previous work we reported that the Y acts as a reactive element, blocking the Fe and C diffusion from the substrate [1]. Here we show that the Y content is critical and depending on the Al content, different behavior is obtained. The highest oxidation resistance and best thermal stability is obtained for the CrAlN coating with 16 at.% Al and 2.9 at. % of Y content, where the initial nanostructure and the cubic phase (fcc-CrAlN) was retained, and a thin (Cr,Al)2O3 oxide protective scale was formed. At lower Y content (1.2 at.%) the iron diffused along the coating arriving to the surface where gets oxidized. Higher Y amount (4.6 at.%) avoided the iron diffusion but a thicker oxide scale is formed with new oxide phases, and the initial fcc-CrAlN phase is partially transformed to Cr7C3. The increment of Al content up to 25 at.% with Y concentration of 2.6 at.% presented a good oxidation resistance at 1000ºC but new phases (h-AlN and Cr-Fe) were formed. The coating with the same Al content but with higher amount of yttrium (5.7 at. %) is completely oxidized.

Authors : Meneka Banik, Rabibrata Mukherjee
Affiliations : Instability and soft patterning laboratory, Department of Chemical Engineering, Indian Institute of Technology Kharagpur, Kharagpur ? 721302, India

Resume : Self organization of colloidal particles has many applications, particularly in fabrication of solar cells with advanced light management strategies. We report a simple, facile spincoating based approach for fabricating two dimensional colloidal crystals with hexagonal and non hexagonal close packed (HCP) arrays with organic as well as inorganic colloidal particles on flat and nano patterned substrates, respectively. Appropriate amounts of surfactant molecules are added to the colloidal dispersion ahead of spin coating to ensure the formation of the HCP patterns. The non-HCP arrays are fabricated by spin coating the particles onto soft lithographically. The substrate patterns impose directionality to the particles by confining them within substrate grooves during spin coating, thereby breaking the hexagonal close packed symmetry into structures that are commensurative with the substrate patterns. Parameters like coating speed, dilution of the colloids, amount of surfactant added and volume dispensed provide a control over the formation of HCP as well as the number of layers deposited. We have also developed a novel technique by which the HCP as well as non-HCP array of the colloidal particles can be transferred to planar as well as non-planar surfaces. For this purpose the colloidal arrays are fabricated on a sacrificial PMMA layer which is subsequently degraded by UV exposure, resulting in transfer of the particles onto any other substrate, including non-planar, curves and rough surfaces. This allows the colloidal structures to be transported across substrates irrespective of their surface energy, wettability or morphology. Since the particle array is transferred onto a substrate, without exposing it to any kind of chemical or thermal environment, it can be utilized for placing particles on top of thin film solar cells for improving their absorption efficiency, without subjecting the completed cell to any further solution processing.

Authors : Jau-Yu Chiou, Yong-Hsiang Peng and Jiang-Jen Lin
Affiliations : National Taiwan University

Resume : A systematic approach of using poly(oxyalkylene)-amine-salt terminated 2,2-bis(4-hydroxyphenyl)propane epoxy oligomers for modifying the layered silicate clays has led to the organoclays with different surfactant properties. The pristine layered structure of natural clays were organically intercalated into basal spacing from 12Å to 100Å and even exfoliated to form randomized thin layer silicate platelets by the amine-oligomers as the first step. These organoclays were characterized by X-ray diffraction and shown their expanded basal spacing up to 100 Å and even randomized into featureless, confirmed by TEM examination. Furthermore, the removal of the amine-oligomers left the hydrophilic randomized thin layer silicate platelets in water phase in the second step. The balance of organic amine-oligomers and inorganic silicate platelets in the structure led to the amphiphilic property. The amphiphilic nature was evidenced by their ability of lowering the surface tension at the water–air interface. The platelet ionic charges were analyzed by zeta potential measurement showing a pH-dependent charge species existed on the surface of the random platelets and the demonstration of charge reverse properties depending on pH. The extremely stable emulsions can be formed for the clay–amine suspension, suggesting the practical uses for pigment dispersion in coating applications.

Authors : Marcela Elisabeta Barbinta-Patrascu(a), Stefan Marian Iordache(b), Ana Maria Iordache(b), Nicoleta Badea(c), Camelia Ungureanu(c), Mihaela Bacalum(d), Florina Lucica Zorila(d), Ioan Stamatin(b)
Affiliations : (a)University of Bucharest, Faculty of Physics, Department of Electricity, Solid-State Physics and Biophysics, 405 Atomistilor Street, PO Box MG-11, Bucharest-Magurele, 077125, Romania (b)University of Bucharest, 3Nano-SAE Research Center, PO Box MG-38, Bucharest-Magurele, Romania (c)University “Politehnica” of Bucharest, Faculty of Applied Chemistry and Materials Science 1-7, Polizu Str., 011061, Bucharest, Romania (d)Horia Hulubei National Institute of Physics and Nuclear Engineering - IFIN HH, IRASM Multipurpose Irradiation Facility, Magurele, Ilfov, Romania

Resume : This study aimed to design hybrid structures based on green nanosilver, bio-polysaccharides, and biomimetic membranes, by using a “green” bottom-up approach. Living plant material was employed to prepare silver nanoparticles. Chlorophyll a embedded in the artificial lipid bilayers was used as optical sensor to monitor the formation of biohybrids. Modern biophysical methods (UV-Vis absorption and emission spectroscopy, AFM, DLS, zeta potential measurements, antioxidant and antimicrobial assays) were used to characterize these bio-based nanocomposites. The obtained biohybrids exhibited high antioxidant activity (checked by chemiluminescence method), and also strong biocidal properties against E.coli, E. faecalis and S. aureus, thus they could be used in biomedical applications as protective biocompatible coatings.

Authors : Lokesh Rana, Reema Gupta, Monika Tomar, Vinay Gupta
Affiliations : Department of Physics and Astrophysics, University of Delhi, Delhi-110007, INDIA; Department of Physics and Astrophysics, University of Delhi, Delhi-110007, INDIA; Physics Department, Miranda House, University of Delhi, Delhi-110007, INDIA; Department of Physics and Astrophysics, University of Delhi, Delhi-110007, INDIA;

Resume : Surface acoustic wave (SAW) devices has been the most suitable platform for the fabrication of any kind of sensor in the last decade. Device properties including cost effectiveness, small size, high sensitivity and wireless detection are grabbing the attention of the researchers towards the realization of SAW sensors. Commercial SAW devices are being exploited successfully for sensing harmful radiations, toxic gases and biological analytes after integration with suitable sensing layer. Since NO2 is toxic gas and is emitted continuously from vehicles and factories, it needs to be monitored continuously. There are few reports in the literature showing NO2 gas sensor based on commercial SAW filters, but with low sensitivity. In order to improve the sensitivity, SAW resonator could be exploited where acoustic energy is confined yielding low losses. The present work reports the fabrication details of 100 MHz SAW resonator based on ST cut Quartz. Reflectors are placed on both sides of interdigital transducers to confine the acoustic energy on the device surface by forming standing waves. Subsequently PZT thin film has been deposited by pulsed laser deposition as a sensing layer over the fabricated SAW resonator. Shift in resonator frequency was measured precisely for varying concentration of NOx gas. The calibration curve was found to be linear which is advantageous for integrating with electronic circuitry for handheld wireless sensing device.

Authors : Avneet Singh, Anjali Sharma, Monika Tomar, Vinay Gupta
Affiliations : Department of Physics and Astrophysics, University of Delhi, Delhi, India; Physics Department, ARSD College, University of Delhi, Delhi, India; Physics Department,Miranda House, University of Delhi, Delhi, India; Department of Physics and Astrophysics, University of Delhi, Delhi, India

Resume : Carbon monoxide (CO) is a colourless, odourless and tasteless gas and is known as silent killer because of its highly toxic nature. It enters into the bloodstream and combines with haemoglobin to form carboxyhaemoglobin, which makes the blood unable to carry oxygen that destroys the human body?s cells and tissues. Thus, there is an urgent need of highly sensitive and selective sensor for the detection of CO gas. Gas sensing phenomenon is strongly influenced by the surface area and morphology of the sensing layer. In this context, nanostructured Zinc Oxide (ZnO) thin film is the best suited material for detection of harmful gases. In the present work, ZnO thin film has been grown by rf sputtering technique in glancing angle deposition (GLAD) configuration. This sensing layer has been deposited on Pt inter digital electrodes (IDEs) patterned glass substrates using a metal Zn target in a mixer of Ar and O2 (1:1) gas ambient. X-Ray diffraction study reveals that the sensing films are highly c-axis oriented and having well defined reflection corresponding to (002) plane of ZnO. The AFM image confirms the formation of highly porous and columnar structures. ZnO nanostructures grown at a GLAD angle of 70° exhibit sensing response of about 372 at a relatively lower operating temperature of 130?C toward 500 ppm of CO gas. The sensor is found to exhibit fast response (46s) and recovery (359s) speeds with high selectivity towards detection of CO.

Authors : Leonardo Mathias Leidens, Ângela Elisa Crespi, Fernando Alvarez, Carlos Alejandro Figueroa
Affiliations : Universidade de Caxias do Sul – UCS and CAPES – Ministério da Educação, Brazil; Universidade de Caxias do Sul – UCS and CAPES – Ministério da Educação, Brazil; IFGW-UNICAMP, Brazil; Universidade de Caxias do Sul – UCS and Plasmar Tecnologia, Brazil

Resume : Diamond-like carbon thin films (DLC) can develop properties such as ultra-low friction coefficient and low wear rates. One of the biggest problems of this coating is its poor adhesion in some substrates, such as low-alloys steels. Many efforts are devoted to study alternatives in order to overcome this problem, like different chemical architectures of interlayers. However, the use of silicon-containing interlayers demands high deposition temperatures, which might degrade previous heat treatments . The aim of this work is to investigate an alternative pre-treatment to reach high enough adhesion in low temperature. A hydrogen plasma etching was used at different times and temperatures to perform a selective chemical cleaning of the silicon-containing interlayer, prior to DLC deposition. The samples were produced by EC-PECVD and characterized by SEM, GDOES and adhesion tests. The chemical structure of the interlayer shows a higher content of carbon atoms in the interface, which is a known factor to improve adhesion, at longer times than 4 min. The produced chemical architecture promotes good adhesion of the DLC temperatures as lower temperatures as 85°C when previous works have only reported good results in temperatures up to 300°C. We propose a mechanism to explain the hydrogen etching and analyze the new pathways generated by this work.

Authors : Jihoon Chung, Sukyung Lee, Dongseob Kim, Yong Tae Park, and Sangmin Lee
Affiliations : Chung-Ang University; Chung-Ang University; Korea Institute of Industrial Technology; Myongji University; Chung-Ang University

Resume : A triboelectric nanogenerator (TENG), a renewable energy technology to efficiently harvest mechanical energy into electrical energy, has elicited worldwide attention because of its cost-effectiveness and sustainability. This device utilizes contact electrification which is induced by friction between two dielectrics with triboelectric polarity to produce electricity from wasted mechanical energy. Recently, the TENG was developed using water-solid contact electrification, which used water as dielectric itself and significantly reduced the friction damage between two materials. In this study, we developed a cylindrical water triboelectric nanogenerator which controls the water flow by fabricating patterned hydrophobic/-philic surface with polytetrafluoroethylene (PTFE) nanocoated surface and anodized aluminum oxide nanopores. As a first report, this study demonstrates new design of fully packaged water-solid contact TENG, called cylindrical water triboelectric nanogenerator (CW-TENG), which has a complete packaged design to generate multiple output in single rotation through patterned surface. CW-TENG can be integrated with multiple generating hydrophobic/-philic generating units in single TENG device without occupying extra space for installation. Furthermore, this study is the first to demonstrate possibility of using hydrophilic surface as additional energy harvesting device as well as water reservoir in a packaged design. Until now, hydrophilic surface was only considered as incompatible element for TENG because water volume on the hydrophilic surface remains after the first contact. The rotating design pushes water on the hydrophilic surface constantly to force the water volume change to induce electrical potential difference between two surfaces. In addition, this study demonstrates analysis of the electrical energy generation by water volume change on the hydrophilic surface with computational dynamic simulation. The electrical potential difference between water and the electrode is shown to increase as the water volume change is increased. Utilizing this new result and analysis, various TENG design using hydrophilic surface can be developed for practical use. In this design, the super-hydrophobic surface TENG generates open-circuit voltage (VOC) of 7 V and closed circuit current (ICC) of 50 nA, and hydrophilic surface TENG can produce VOC of 2 V and ICC of 60 nA. With more super-hydrophobic and hydrophilic patterned electrode inside this device, the total power generated by the device is estimated to be multiplied. Thus, with this research will provide a potential solution of energy harvesting using water flow and self-powered system.

Authors : I.A. Veselova, M.I. Makedonskaya, O.E. Eremina, A.V. Sidorov, S.N. Kalmykov, T.N. Shekhovtsova, E.A. Goodilin
Affiliations : Lomonosov Moscow State University, National Research Centre "Kurchatov Institute"

Resume : The catecholamines such as dopamine, norepinephrine, and epinephrine are the principal neurotransmitters in the sympathetic nervous system. Catecholamines and their metabolites are considered to be important markers of socially significant diseases such as atherosclerosis, diabetes, coronary heart disease, carcinogenesis, Alzheimer's and Parkinson's diseases. Currently, neurotransmitters can be studied via electrochemical and chromatographic techniques that provide characterization and quantification, although these techniques can only provide crude spatial information. Besides, the difficulty of catecholamine determination in biological materials is associated with their low normal concentrations (about 1 nM) in biomaterials, which may become even one more order lower because of some disorders. In addition, in blood they are rapidly oxidized by monoaminooxidases from thrombocytes and, for this reason, the determination of neurotransmitter metabolism indicators in organism should be very rapid (15?30 min), especially in critical states. Unfortunately, modern instrumental analysis does not offer a complex solution of this problem: despite its high sensitivity and selectivity, HPLC-MS cannot provide sufficiently rapid analysis, while enzymatic biosensors and immunoassays for the determination of the considered analytes lack sufficient sensitivity and reproducibility. Fluorescent and SERS-sensors remain a compelling technology for approaching the general problem of selective neurotransmitter detection. In recent years, a number of catecholamine sensors have been reported including RNA aptamers, fluorescent ribonucleopeptide (RNP) complexes, and boronic acid based synthetic receptors and the sensor operated in a turn-off mode. In this work we present the fluorescent and SERS turn-on sensor systems based on the bio- or chemorecognizing nanostructured films {chitosan-Tb/Eu/Cu-nanoparticles-indicator reagents} that allows for the selective recognition, visualization and sensing of the above mentioned catecholamines on the level of nanomolar concentration in biomaterials (cell cultures, tissue etc.). It was (1) developed optically transparent porous films and gels of chitosan; (2) ensured functionalization of the surface by molecules-«recognizers» (by impregnation and immobilization of components of the indicator systems: biorecognizing and auxiliary reagents); (3) performed computer simulation for theoretical prediction and interpretation of some properties of the developed materials and obtained analytical signals in biomaterials. We are grateful for the financial support of this research from Russian Foundation for Basic Research (grants no. 15-03-05064 a, and 15-29-01330 ofi_m).

Authors : Nuri Burak Kiremitler, Sami Pekdemir, ?lker Törün, Serdar Önses
Affiliations : Erciyes University Department of Material Science and Engineering Erciyes Universty Nanotechnology Research Center (ERNAM)

Resume : Patterning of functional nanomaterials on surfaces at nanometer length scales are critically important to many applications and scientific fields. Here we show far field (ES) and near field electrospinning (NFES) techniques can be used for generating patterns of polymer brush nanoribbons (PBNR) as small as 100 nm on surfaces as a low-cost simple process as called by us Electrospin Nanolitography (ESPNL). In this study we demonstrate two unique approaches to fabricate PBNRs aid of electrospun nanofibers. At first approach, polymers which can be graft as polymer brushes on surfaces are directly electrospun on surface. Polymer fibers on the surface through thermal annealing followed by washing leads patterns of PBNRs. At second and more effective approach, we use electrospun nanofibers masks on top of a substrate grafted polymer brushes. The oxygen plasma etching and washing of the substrate leads to patterns of PBNRs. PBNR arrays can be aligned by rotating drum collector. Furthermore desired geometric patterns of PBNRs were fabricated easily by using NFES technique. These alignment or geometrically designed patterns then be used to selectively localize nanomaterials such gold and silver nanoparticles. Results of our study show that the width of the PBNRs can be controlled with the fiber as well as ES and NFES conditions. We fabricated patterned PBNRs with less than 50 nm. To demonstrate an example of possible application of this technique, Au NPs with different size and shape were selectively immobilized on PBNRs to generate heterostructures. These structures performed strong surface enhance Raman scattering effect (SERS) for plasmonic and signal sensing applications. Also patterned Au nanoribbons with different size and shape can also use as nano cables for electronic industry. To sum, the scalability and simplicity of ESPNL hold great promise in patterning of a broad range of functional nanomaterials for different application related nanolithography techniques. With our technique not only PBNRs and also functional materials such as graphene, polydopamine or coated thin films can be fabricated and also patterned in desired shape with high resolution as small as 100 nm easily. Also as we shown functional nanoparticles can be selectively immobolize on these nano ribbons for wide range of applications.

Authors : Fotini Pappa, Varvara Karagkiozaki, Stergios Logothetidis
Affiliations : Nanomedicine Group, Laboratory for “Thin Films, Nanobiomaterials, Nanosystems and Nanometrology” (LTFN), Department of Physics, Aristotle University of Thessaloniki, Greece

Resume : Nanomedicine provides a new paradigm of rational delivery of therapeutic and diagnostic agents to the diseased sites that renders site specific therapy. In the case of atherosclerosis, the detection of vulnerable plaques that are prone to rupture is a challenge that needs to be addressed for the reduction of incidence of heart attack and stroke in younger patients. This talk focuses on Nanomedical targeting strategies in atherosclerosis and possible molecular targets within the plaque to regress its progression. An overview of the diversity of the nanoparticulate systems with surface ligands targeted for macrophages and other cell types of the vulnerable plaques will be given in line with drug delivery systems that elicit anti-inflammatory/- proliferative drugs. The Bioelectronics strategy encompasses the application of conductive polymers and devices that due to their high ionic and electronic conductivity can merge as translators between the ‘nanoworld’ of the cells with the implant interface. Tissue regeneration activities are essential for dealing with the late stent thrombosis of drug eluting stents (DES) that it is mainly caused by delayed endothelialisation. The new perspectives of organic bioelectronics and their marriage with nanomedicine aimed for atherosclerosis will be highlighted providing intelligent solutions for its accurate diagnosis and effective therapy. Acknowledgements This work has been supported by the EU FP7-REGPOT 2011-1 Project ROleMak, GA 2860 an

Authors : A. Grunin, A. Goikhman, K. Maksimova; A. Gloskovskii
Affiliations : Immanuel Kant Baltic Federal University, 236041 Kaliningrad, Russian Federation DESY Photon Science, Deutsches Elektronen-Synchrotron, 22603 Hamburg, Germany

Resume : Over the last decades a lot of attention was devoted to Ni-Mn-In Heusler alloys, because of their intriguing properties important for various applications, such as caloric effects, theoretically predicted high spin polarization, magnetic-induced first-order phase transition etc. Many of these properties originate from the martensitic transition. Due to the possibility of using this effects for different applications a lot of scientific and technological attention is attracted now to the low-dimensional materials like thin films. Therefore, it's very important to determine structural and magnetic properties changing upon the decreasing z-dimension of the material from bulk to few atomic layers film. Martensitic transition is a first-order reversal structural transition from high temperature cubic phase to martensitic phase with lower symmetry. In this work the polycrystalline Heusler alloy thin films with Ni52Mn48-xInx (12< x< 16) composition and thicknesses about 50 nm were grown by pulsed laser deposition. The magnetic attributes of martensitic transition, observed by PPMS, were found in a much wider temperature interval (about 200 K), than structural ones, studied by X-ray diffraction (about 90 K only). The similar broader temperature range of transition is observed for electronic structure investigation of the valence band, provided by hard X-ray photoelectron spectroscopy on P09 beamline at PETRA III synchrotron source. The thermomagnetic investigations are concluded as more accurate approach for martensitic transition characterization for thin films.

Authors : Shang-Chieh Huang, Hsueh-Shih Chen
Affiliations :;

Resume : Quantum dots (QDs) have been used increasingly to achieve broader color gamut and enhance power efficiency in displays due to their narrow emission band and high photoluminescence quantum yield (PLQY). The most common application form of QDs in display nowadays is to incorporate QDs in a polymer film that used as a luminescent down-shifting layer in liquid crystal displays (LCDs). In this study, we fabricate uniform QD/polymer with a high light-conversion efficiency (LCE). We have achieved good QD dispersion in the polymer to retain its high PLQY and improve the stability. We have also investigated the effects of scatter particles (SCs) with different sizes on the optical properties and efficiency of the QD/polymer films. We found that the scattered light from the film increases with the increasing of SCs amount in the polymer matrix; whereas the LCE of the film drops after reaching a certain SCs concentration in the matrix due to the saturation of the light path.

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New energetic plasma processes and related advanced coatings for energy conversion, saving and storage : Sven Ulrich + T. Polcar
Authors : Sven Ulrich, Klaus Seemann, Harald Leiste, Michael Stüber
Affiliations : Karlsruhe Institute of Technology – KIT, Institute for Applied Materials – IAM, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany

Resume : All-solid-state thin-film lithium ion batteries have a great application potential, in particular for the use in microsystem technologies, such as MEMS, CMOS memories, medical implants and devices, smart cards, skin patch, RFID, wearables, E-textiles, smart phones, due to their high power density and high safety. All-solid-state lithium ion batteries comprise three main parts, the cathode, solid state electrolyte, and anode, in addition to two art collectors for the cathode and anode, respectively. Besides the material properties of individual components, the contact of the current collectors to the anode and cathode, as well as the interfaces between the cathode, anode and solid state electrolyte are of crucial importance for the battery performance. This article provides an overview of the current research status, highlighting the individual battery components in terms of their material selection, constitution, microstructure as well as the physical, chemical and electrical properties. Important analysis techniques, particularly in-situ analysis, and simulation methods are exemplarily presented. The challenges in up-scaling, deposition on flexible substrates such as metal sheets, polymer substrates and ultrathin glasses and the possibility of the realization of a roll to roll process will also be discussed.

Authors : S M Iftiquar and Junsin Yi
Affiliations : College of Information and Communication Engineering, Sungkyunkwan University, Suwon, 440-746, Korea

Resume : Hydrogenated amorphous silicon material has been investigated extensively for its application in thin film solar cells. However, defects, stability and reproducibility are few of the important issues for its large scale application in commercial devices. A combinatorial effect of the parameters like optical absorption, photo-electric sensitivity, carrier mobility-lifetime product, optical gap, atomic structure of the material, defect density etc also is thought to limit the maximum achievable device efficiency. We investigated effect of a pair of complementary material parameters to determine maximum achievable device efficiency. In this regard defect density and thickness of active layer were found to form a complementary pair with which a maximum device efficiency is achievable. In our investigation, the defect densities of solar cell active layers were in the range of 4×1015 to 8×1017 cm-3, and its thickness were in the range of 25 to 3000nm. We observed that the highest available device efficiency (Eff) of the solar cells and defect density (Ndd) of the active layers are related by Eff =0.544 –0.0278 Log10(Ndd). For example, a solar cell with 10% efficiency can be obtained if defect density of active layer, Ndd = 8.9×1015 cm-3 whereas a 20% efficient solar cell can be obtained if the Ndd = 1.0×1012 cm-3.

Authors : G. Croizier, P. Martins, M. Le Baillif, R. Aubry, S. Bansropun, M. Fryziel, N. Rolland, A. Ziaei
Affiliations : G. Croizier ; P. Martins ; M. Le Baillif ; R. Aubry ; S. Bansropun ; A. Ziaei Thales Research and Technology, F-91767, Palaiseau Cedex, France M. Fryziel ; N. Rolland Institut d’Electronique de Microélectronique et de Nanotechnologie, F-59652, Villeneuve d’Ascq Cedex, France

Resume : This paper reports a study over a wide range of high-K dielectric materials deposited by different techniques for high power RF MEMS switches applications. For capacitive switches, dielectric material optimization is one solution to further increase power handling and reliability alongside design improvement. For electrostatic MEMS switches under high RF power (>20W), the dielectric material has to withstand high electric field (>4MV/cm). Through dielectric study, we intend to introduce promising materials in order to go beyond demonstrated power handling of 20W with reliability up to 10^7 cycles [1]-[2]. E-beam evaporation with Ion Assisted Deposition and Atomic Layer Deposition were studied based on three High k materials : Al2O3, HfO2 and TiO2. These materials were compared to Si3N4 Plasma Enhanced Chemical Vapor Deposition, as reference material. Crossed electrical characterizations on MIM capacitors and physical analyses were performed on all materials. This study shows that electrical properties of ALD materials are in good agreement with Mc Pherson & Al. trend [3] regardless of allowed oxygen excess and carbon contamination. This means that high-K materials can be tuned using ALD depending on application specifications. ALD HfO2 insulators were identified as promising for high power RF applications. Preliminary tests to integrate thermal ALD HfO2 in RF MEMS switches show that it is possible to further enhance DC stress handling without RF performance degradation. References [1] H.-H. Yang, H. Zareie, G. M. Rebeiz, Journal of Microelectromechanical Systems 24, 599 – 607 (2015) [2] A. Ziaei, S. Bansropun, P. Martins, M. Le Baillif, European Solid State Device Research Conference 2015 (ESSDERC), 153 (2015) [3] J. Mc Pherson and Al., Appl. Phys. Lett. 82, 2121 (2003).

Authors : A. Hardy, Marlies K. Van Bael
Affiliations : UHasselt, Institute for Materials Research, Inorganic and Physical Chemistry and imec, division imomec, Agoralaan, Diepenbeek, Belgium

Resume : Coating non-planar microstructured surfaces is highly challenging, especially when a high degree of conformality is required. Typically, such conformal coatings are championed by atomic layer deposition (ALD). However, ALD struggles to reach a thickness of several tens of nanometers, because of the long deposition times. Here, we present ultrasonic spraycoating of solution precursors, which achieved uniform coatings on structures with aspect ratio 10. Since such precursors can be synthesized for most metal ions, a wide range of materials is accessible. Here, we focused on anodes (TiO2, LTO, WO3), cathodes (LMO), solid electrolytes (LLT), as well as current collectors (ITO) for the fabrication of a 3D thin film lithium ion battery. Insights into the spraycoating process and the precursor chemistry explained the success of the method. The properties of the individual battery components (crystal structure, morphology, CV curves, charge-discharge profiles,…) and the specific material’s integration issues will be discussed. The capacity enhancement finally reached a factor 4. This remains unrivaled at the moment, also for vacuum based deposition methods such as CVD. IWT project SBO SOSLION and UHasselt (BOF-IOF) are acknowledged for financial support. E. J. van den Ham, et al. ACS ENERGY LETTERS, 2016 1, p.1184-1188 G. Maino, et al. J. Mater. Chem. A, 2016, 4, p. 18457-18469 E. J. Van Den Ham, et al. RSC Advances 2016, 6, p. 51747-51756

Authors : Maryna Bilokur, Angus Gentle, Matthew Arnold, Geoff Smith, Michael Cortie
Affiliations : Institute of nanoscale technology (INT), University of Technology of Sydney (UTS)

Resume : Solar photo thermal conversion of photovoltaic devices at elevated temperatures can be enhanced by exploitation of thermally stable spectrally selective coatings. One of the critical approaches is designing nanocermet layers as a part of a multilayer stack with a stable dielectric matrix and encapsulated metallic nanoparticles with low thermal diffusion. In our study, ultrastable TiAlN and AlN semiconducting compounds were synthesised by magnetron sputtering for high temperature solar thermal applications. It is believed that transported fractions of transitional metal into a dielectric AlN matrix can stabilize a newly formed TiAlN alloy and boost thermal tolerance. The dynamic in-situ X-Ray diffraction studies show that single layers of TiAlN and AlN on a tantalum substrate can tolerate the temperature annealing up too 1400K in vacuum ambient with no structural change. No oxidation or interdiffusion reaction with the substrate was observed. High resolution transmission electron microscopy (HRTEM) analysis was conducted to understand the microstructural nature of a solid TiAlN solution with a face centred cubic (FCC) structure. Optical modelling using WVASE software (J.A. Woollam Co.) and experimentally determined optical constants of the deposited thin films demonstrates that a TiAlN/AlN based multilayer is a great candidate for solar selective absorption, with an integrated solar absorption ranging between 90% and 97%. This implies the potential use of superior thermally stable TiAlN/AlN based spectrally selective multilayer coatings to achieve higher efficiency in thermo-photovoltaic devices.

Authors : Anne-Charlotte Amiaud, Aude Leuliet, Julien Nagle, Brigitte Loiseaux, Paolo Martins, Raphaël Aubry, Stéphane Holé
Affiliations : Thales Research & Technology, Palaiseau, France ; LPEM – CNRS, Sorbonne Universités, UPMC Univ. Paris 6, PSL Research University, Paris, France

Resume : The reliability of electronic components is affected by dielectric layer aging. When component sizes are reduced insulator films are subject to high applied electric fields (MV/cm) and charges can be injected. These charges modify component properties and can lead to system failure. A better dielectric charging understanding enables charge accumulation control. In this work dielectric charging process in capacitive structures under bias voltage is investigated. We particularly focus on the case of capacitors with silicon nitride dielectric thin layers. A one dimensional dielectric charging model is presented including free and trapped carrier transport. This is based on the resolution of both Maxwell-Gauss and charge continuity equations. Several relevant charge transport mechanisms are taken into account. Trap Assisted Tunneling effect and Schottky injection are the interfacial mechanisms, trapping and detrapping mechanisms (including Frenkel-Poole effect) and space charge limited current are considered for bulk mechanisms. Electric field, current and charge carrier distribution can be calculated in the whole dielectric layer as a function of time. Simulated currents show the same order of magnitude as measured currents for different applied electric fields. Adding the discharging process, this model becomes a forecasting tool for component lifetime. The proposed model can be used as a simulation tool to choose materials according to device performances targeted.

Authors : Lv Junjun, Wang Wanjun, Guo Fei, He Xiaodong
Affiliations : Institute of Chemical Materials, CAEP

Resume : Nanomaterials are a topic of increased interest for many applications. Reactive Al/Ni multi-layer thin film can produce rapid bursts of heat and light through a homogeneous or self-propagating reaction. The exothermic reactions can be ignited using pulses of electrical, mechanical, optical, or thermal energy. In this paper, Al/Ni nano multi-layer thin film was fabricated using magnetron sputter deposition. Transmission Electron Microscope(TEM) was used to characterize the section configuration of the thin film. Then, taking advantage of standard photolithography and developing technology, a type thin film high voltage switch was fabricated. The switch was composed by two main electrodes and a trigger electrode, and paraxylene film was used as insulating medium between main electrodes. Scanning electron microscope (SEM) and stylus profiler was employed to ascertain multi-layer structure and dimension of the switch. Then, we discussed the discharge characterization of the Al/Ni thin film switch using electrical and laser energy as a trigger method. We carefully examined the delay time, the peak current of the discharge circuit under different charging voltage and different trigger method. The switches in our work were connected to a capacitive discharge circuit and tested, and a 0.22 µF capacitor was charged to a certain volts. One pulse trigger voltage which was applied between trigger electrode and ground of the circuit was employed to initiate the actuation of the switch. DPO3054 oscillograph and a Rogowski coil current transformer were utilized to monitor the current waveform of the circuit. Compared with commercial stereo spark gap switch, because the energetic thin film was utilized to cause the break-over of the high voltage switch. The switch could be triggered by a voltage as low as 50V, which obviously could reduce the volume of trigger circuit. When the thin film high voltage switch was connected into a capacitive discharge unit(CDU), the discharge circuit had lower inductance and higher resistance. Using laser trigger method, the current-carrying ability of the switch was enhanced. The peak current is about 2700 A when the charging voltage is 2500 V. In order to understand discharge process further, the high-speed photography (HSP) technique and spectral temperature measurement technology were applied to the investigation of discharge process of the witch. Ablation of the electrodes was analyzed using metallographic microscope.

Authors : M.J. Milla, F. González-Posada, L. Cerutti, F. Barho, M. Bomers, E. Tournié and T. Taliercio
Affiliations : M.J. Milla, F. González-Posada, L. Cerutti, F. Barho, M. Bomers, E. Tournié and T. Taliercio Université de Montpellier, IES, UMR 5214, F-34000, Montpellier, France; CNRS, IES, UMR 5214, F-34000, Montpellier, France

Resume : Plasmonic nanostructures have been proposed as potential materials for the development of biochemical sensors and surface-enhanced spectroscopies. Noble metals nanostructures have been generally used for surface plasmon technology in the visible, however they present limitations for longer wavelength applications. Highly doped semiconductors (HDSC) have been recently proposed as potential materials for the development of sensing devices in the mid-IR, molecule fingerprint region. In particular, the system based on 1-dimensional (1-D) Si-doped InAsSb/GaSb nano-antennas have proved to outperform gold standards in this spectral range and demonstrated surface plasmon resonance (SPR) sensing. SPR and surface enhanced infrared absorption (SEIRA) are compatible techniques for sensing in the mid-IR. Their combination enables the accurate identification of surrounding molecules. In this work, we demonstrate SEIRA sensing of 1-D Si:InAsSb/GaSb nano-antennas devices by using a SiO2 layer. The nano-antennas were designed to have a LSPR peak at the energy to reach the maximum electric field exaltation. Different SiO2 thickness were deposited on top of the nanostructures by e-beam physical evaporation. We report a clear dependence of the SEIRA sensing on the thickness of the SiO2 and the control of the nano-antennas fabrication to obtain the maximum enhancement of the molecule IR absorption, and thus to improve the sensing device efficiency.

Authors : E. G-Berasategui, N. Bolaños, L. Mendizábal J. Barriga
Affiliations : IK4-TEKNIKER, Research Centre, c/ Iñaki Goenaga, 5, 20600 Eibar, Guipuzcoa, Spain

Resume : Transparent conducting oxides (TCO), acting as transparent electrodes, are essential components in the basic structure of a large number of electronic devices as flat panel displays, touch screens, photovoltaic cells, lighting emitting diodes or electrochromic systems. The trade-off between transparency and conductivity in these materials is a major bottleneck towards higher device performance. Indium tin oxide (ITO) is the most established transparent conductive film in the market as currently presents the best optoelectronic properties. The current solution to further improve conductive properties of these materials is to deposit some metallic grids or nanowires on surface of the TCOs but transparency is always decreased and different manufacturing processes are combined. In this work, Ag nanoparticles deposited by gas aggregation sources has been incorporated into ITO layers deposited by DC pulse magnetron sputtering improving the conductivity of the layers while keeping transmission values by a simple one step process. The study of the composite optoelectronic properties has been carried out as a function of the process parameters to correlate those properties with the composition and morphology of the layers. The influence of the nanoparticles density has been carried out to optimise optoelectronic properties. This hybrid electrode is demonstrated to have a 5 times smaller sheet resistance compare to a single TCO layer, while maintaining high light transmission in a wide wavelength range.

Authors : R. Romero, F. Martin, J.R. Ramos-Barrado, D. Leinen
Affiliations : Lab of Materials y Surfaces, Applied Physics & Chemical Engineering Departments, University of Malaga, Faculty of Science, E-29071 Málaga, Spain

Resume : Ag-ZrO2 cermet coatings on aluminized steel sheet have been obtained by a step by step approach to a multilayer system using uniquely the chemical spray pyrolysis technique. First single layers of metallic silver particles and zirconia were prepared on aluminized steel sheet (AS) and spray parameters were optimized. Then cermet coatings with different layers (ZrO2/Ag/AS; ZrO2/Ag ZrO2/AS; ZrO2/Ag ZrO2/Ag/ZrO2/AS) were prepared and studied with respect to their functional application for solar thermal devices. As evidenced by SEM and AFM studies, silver nanoparticles with a size distribution of 10 to 50 nm imbedded in zirconia can be obtained with a simple air pressure spray technique. Solar parameters as solar absorptance (AM 1.5) and thermal emittance (373K) were determined showing to reach 90% and 20% respectively. Layer thicknesses and chemical compositions were investigated with C60 XPS depth profiling showing small amounts of silver at the top most surface of the coatings and silver particle size distributions in agreement to the observations made by SEM/AFM. The stability of the coating system was evaluated for harsh environment with cyclic voltammetry and amperometry and outdoor exposure measurements.

Authors : Tuomas Hänninen 1, Susann Schmidt 1, Ivan G. Ivanov 2, Lars Hultman 1, Hans Högberg 1
Affiliations : 1 Thin Film Physics Division, Department of Physics, Chemistry and Biology (IFM), Linköping University, SE-581 83, Sweden 2 Semiconductor Materials Division, Department of Physics, Chemistry and Biology (IFM), Linköping University, SE-581 83, Sweden

Resume : Amorphous silicon carbonitride (SiCN) thin films were deposited by reactive high power impulse magnetron sputtering (HiPIMS) from a pure Si target in argon/nitrogen/acetylene plasmas. The influence of the acetylene flow (0-50 sccm), substrate temperature (no additional heating-510 °C), HiPIMS pulse frequency (200-1200 Hz at an average target power of 1200 W), and negative substrate bias (60-200 V) on the resulting film properties were investigated. For all processes, the nitrogen-to-argon flow ratio was set to 0.28 at a pressure of 400 mPa, while the pressure was let to increase as acetylene was introduced into the chamber. X-ray photoelectron spectroscopy shows an increasing film carbon content from ~9 at.% to ~90 at.% as the acetylene flow is increased from 2 sccm to 50 sccm. Simultaneously, the film density decreases from ~3.0 g/cm3 to ~1.6 g/cm3. For films with C contents ≤20 at.%, hardness values between 21 and 22 GPa were measured by nanoindentation, resembling a similar hardness as the SiN reference sample. These films show dense and featureless morphologies when viewed in cross-sectional scanning electron microscopy. As the C contents increase, an increasingly columnar morphology is observed and the hardness values decrease to a minimum of ~5 GPa. The results indicate that low acetylene flows can be used as the C-source for SiCN films deposited by HiPIMS, while not compromising the desirable mechanical properties of SiN.

Authors : Victor Chang, Bruno Camino, Nicholas M Harrison, Tim Noakes
Affiliations : Bruno Camino; Nicholas M Harrison; Imperial College of London; Tim Noakes; STFC Daresbury Laboratory

Resume : Free electron lasers (FELs) are the 4th generation of light source for the study of structural and time resolved properties of material and molecular. FELs are a pulsed, coherent, tuneable and monochromatic light source that works from THz to X-rays in time scales of fs and six order of magnitude brighter than the 3rd generation of light source such as synchrotron. In FELs, the quality of the emitted radiation depends on the quality of the electron beam as they are a single pass device. Therefore, the improvement on the design and efficiency of the photocathode as the source of electrons are a key factor. However, the emission mechanism and how this depends on the material properties is not clear. In this work, an approach to the photoemission of electrons is studied with ab initio calculations and an extension of Spicer’s three steps model. This approach is able to correlate directly the photoemission to the electronic, atomic and chemical structure of the surface. Surface engineering of photocathodes show promising possibilities in the control of their properties. It has previously been demonstrated that thin metal oxide films can generate surface localised states and alter the workfunction of the surface. A systematic understanding of these interactions is therefore a promising approach to engineering highly efficient photocathodes. Our approach, suggest that metal thin oxide over metal photocathodes can be used to increase the quantum efficiency of materials.

Poster session 3: Nanoscience, Nanotechnology and Nanostructured Materials : Philippe Steyer + F. Vaz
Authors : Marouan Khalifa, Malek Atyaoui, Hatem Ezzaouia
Affiliations : Semiconductor and Advanced Technology Nanostructured Laboratory, Research and Technology Centre on Energy, Borj-Cedria Science and Technology Park, BP 95, 2050 Hammam-Lif, Tunisia

Resume : The elaboration and deposition effect of silver nanoparticles on optical and electrical properties of porous silicon layer was investigated. The silver nanoparticles were deposited on porous silicon layer using a thermal evaporation method followed by a thermal treatment at 180°C under nitrogen atmosphere. Photoluminescence and UV_Visible analysis of the treated samples were examined to understand the role of silver nanoparticles. The effect of the deposited nanoparticles on the electrical properties was evaluated by the AC impedance spectroscopy. The results indicate that the formation of the metal nanoparticles is accompanied by enhanced photoluminescence intensity and improved electrical parameters.

Authors : Emrecan Soylemez, Maarten P. de Boer
Affiliations : Emrecan Soylemez, Department of Mechanical Engineering, Faculty of Engineering, Marmara University, Istanbul, 34722, Turkey; Maarten P. de Boer, Mechanical Engineering Department, Carnegie Mellon University, Pittsburgh, Pennsylvania, 15213, USA

Resume : Capillary bridge formation between adjacent surfaces in humid environments is a ubiquitous phenomenon. It strongly influences tribological performance with respect to adhesion, friction and wear. Only a few studies, however, assess capillary dynamics. Here we focus on how capillary nucleation influences adhesion energy dynamically. Microcantilevers adhered to the adjacent surface are used to measure adhesion energy. Our experimental results indicate a logarithmic decrease in average crack healing velocity as energy release rate increases. Our goal is to model those results. We assume that capillary dynamics involve two mechanisms during the evolving of the capillary force: capillary nucleation and capillary growth. We find that by incorporating interface roughness details and the presence of an adsorbed water layer, the behavior of capillary force dynamics can be understood quantitatively. To fully capture the results, however, the theoretical model for nucleation time required an empirical modification. Our model enables significant insight into capillary bridge dynamics, with a goal of attaining a predictive capability for this important microelectromechanical systems (MEMS) reliability failure mechanism.

Authors : S. Gavalas1,2, E. Gagaoudakis1,2, E. Aperathitis1, G. Kiriakidis1,2,3, V. Binas1,2,3
Affiliations : 1 Institute of Electronic Structure and Laser, Foundation for Research and Technology Hellas, 100 N. Plastira str., Vassilika Vouton, 70013 Heraklion, Crete, Greece 2 University of Crete, Department of Physics, 710 03 Heraklion, Crete, Greece 3 Crete Center for Quantum Complexity and Nanotechnology, Department of Physics, University of Crete, 71003 Heraklion, Greece

Resume : Vanadium pentoxide or vanadia (V2O5) is one of the few oxides having versatile redox dependent properties due to the multiple valence state of vanadium and as a result it can be used in numerous applications, such as catalysis, electrochromism and gas sensing. Furthermore, vanadium dioxide (VO2), is a well known thermochromic material, since it undergoes a semiconductor to metal transition (SMT) at a critical transition temperature TC = 68 oC that is close to room temperature. In this work, solution based Vanadium oxides (V2O5 and VO2) nanostructured thin films have been developed by aerosol spray pyrolysis and were deposited on Corning glass substrates. The structure of the films was characterized by X-Ray diffraction (XRD) technique, while Atomic Force Microscopy (AFM) was employed for surface analysis of the films. V2O5 films were tested against ozone showing a change of electrical current of about 1 order of magnitude at 5 ppb ozone concentration. Finaly, V2O5 films were post-annealed in order to take thermochromic VO2 phase. A decrease of IR transmittance of more than 3% at λ = 2500 nm, upon heating.

Authors : Skander Ktifa , N.Yacoubi , H. Ezzaouia
Affiliations : Photovoltaic Laboratory, Research and Technology Centre of Energy,

Resume : The aim of this work is to investigate the influence of Rh6G concentration on optical and thermal properties of nanocomposite porous silicon-Rh6G. Photothermal spectroscopy is carried out in order to determine optical spectra and gap energy of nanocomposite samples which is found to increase with Rh6G concentrations. Photothermal deflection is used to measure nanocomposite thermal conductivity. Nanocomposite thermal conduction is enhanced by the insertion of Rhodamine molecules in the porous matrix. Also, Photoluminescence spectra show an enhancement of energy transfer from porous silicon to nanocomposite band due to Rh6G.

Authors : Nilesh Vats , Stephan Rauschenbach , Wilfried Sigle , Marko Burghard , Klaus Kern, Peter A. van Aken
Affiliations : Max Planck Institute for Solid State Research , Stuttgart, 70569 Germany.

Resume : Single-layer graphene (SLG), as transmission electron microscope (TEM) sample support, offers enormous potential to image nanoparticle, single molecule and ad-atoms at atomic resolution - [1]. Available experimental evidence involving the adsorption mechanism of individual molecules on pristine free-standing SLG is scarce and the resolution of TEM micrograph is limited by low signal to noise ratio. Here, we show that phosphotungstic acid (PTA) molecules have greater affinity to adsorb onto amorphous impurity present on graphene compared to pristine SLG. Furthermore, atomic-scale characterization of the PTA molecule [PW12O40]3- adsorbed on SLG using low-voltage (80 keV) aberration-corrected, high-resolution TEM was performed. This work demonstrates how electrospray ion-beam deposition (ES-IBD) - [2] can be effectively used to land molecules onto ultra-clean SLG - [3] using different landing energies in ultra-high vacuum (UHV) condition. Our study provides first experimental results involving soft landing, adsorption and characterization of individual poly-oxo-metalate (POM) anions onto SLG which can give insight into fabrication of complex two-dimensional materials involving graphene and POM molecules that could find application in electrochemistry and catalysis - [4]. References [1] Nair, R. R. et al., Applied Physics Letters, 97(15), 153102, (2010) [2] Rauschenbach, S. et al., Small, 2, 540-547, (2006) [3] Longchamp, J-N. et al., Journal of Vacuum Science & Technology, B 31, 020605, (2013) [4] Mizuno, Noritaka et al., Chemical Reviews, 98.1, 199-218, (1998)

Authors : J. G. Han,1 B. B. Sahu,1 Y. Yin,1 J. S. Lee,1 and M. Hori2
Affiliations : 1Center for Advanced Plasma Surface Technology (CAPST), NU-SKKU Joint Institute for Plasma Nano Materials (IPNM), Department of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 440-746, South Korea

Resume : The advanced materials process utilizing non-thermal plasmas with a high plasma density enables the synthesis of small-to-big sized Si quantum dots (QDs) by combining low-temperature deposition with superior crystalline quality in the background of an amorphous hydrogenated silicon nitride matrix. The characterization of plasma and atomic radical parameters along with the energy influx from plasma to the substrate during plasma enhanced chemical vapor deposition (PECVD) of Si QD films is presented and discussed. Particularly, relating to the Si QD process optimization and control of film growth, the necessity to control the deposition environment by inducing the effect of the energy of the key plasma species is realized. In this work, we report dual frequency PECVD processes for the low-temperature and high-rate deposition of Si QDs by chemistry and energy control of the key plasma species. The dual frequency plasmas can effectively produce a very high plasma density and atomic H and N densities, which are found to be crucial for the growth and nucleation of QDs. Apart from the study of plasma chemistry, the crucial role of the energy imparted due to these plasma activated species on the substrate is determined in light of QD formation. Various plasma diagnostics and film analysis methods are integrated to correlate the effect of plasma and energy flux on the properties of the deposited films prepared in the reactive mixtures of SiH4/NH3 at various pressures. The analysis reveals that the plasma chemistry plays a crucial role in shaping the QD size with an overall variation from ~ 4 to 11 nm in an amorphous silicon nitride network for the films deposited at various pressures. The present results are highly relevant to the development of the next-generation plasma process for devices that rely on effective control of the QD size and film properties.

Authors : E. C. Romani, S. Nardecchia, C. Vilani *, S. B. Peripolli &, Shaojun Qi +, Hanshan Dong +, F. L. Freire Jr.
Affiliations : Departamento de Física PUC-Rio, Rio de Janeiro, RJ, Brazil ; * Departamento de Engenharia Química e de Materiais, PUC-Rio, Rio de Janeiro, RJ, Brazil; & Centro de Tecnologia SENAI Solda, Rio de Janeiro, RJ, Brazil.
 + School of Metallurgy and Materials, University of Birmingham, Birmingham, UK

Resume : The coating industry has been working to improve surface properties targeting an improvement of corrosion and wear resistances, adhesion, among others. In many cases, nanocoating acting as protective films may prevent future problems and extend the devices lifetime. In this sense, polymer nanocomposites have recently attracted major attention because the synthesis process is cheap and the process to apply on steel substrates is easy. The graphene oxide combined with polymers were revealed an impermeable nanocomposite to gases and liquids and from this perspective have attracted particular interest to application on oil and gas industries. In this work, we report the methodology to produce the nanocomposite film of polyurethane and graphene oxide (GO), as well as reduced graphene oxide (RGO), applied on steel stainless (X80 API 5L). The samples were characterized by optical and scanning electron microscopy (SEM), XPS, Raman Spectroscopy, nanoscratch tests for adhesion behaviour. The dispersion of GO and RGO throughout the composite is also discussed. Corrosion tests reveal that the use of RGO increases the corrosion resistance. 
This work is partially supported by University of Birmingham and by the Brazilian agencies: CNPq and FAPERJ

Authors : W.M. Seidl1, M. Bartosik1,2, H. Bolvardi3, S. Kolozsvári4, P.H. Mayrhofer1,2
Affiliations : 1 Christian Doppler Laboratory for Application Oriented Coating Development, TU Wien, Austria; 2 Institute of Materials Science and Technology, TU Wien, Austria; 3 Plansee Composite Materials GmbH, Germany; 4 Oerlikon Balzers, Oerlikon Surface Solutions AG, Liechtenstein

Resume : The build-up of residual stresses in physical vapour deposited hard coatings can lead to delamination and crack formation when a critical stress value is exceeded. This limits the maximum possible coating thickness. For some applications, however, thick coatings are desired as they often possess superior properties in comparison with their thinner counterparts. It is therefore of uttermost importance to understand, how residual stresses build up and how the stress state can be tailored. In this contribution, we systematically studied the residual stress state of TiAlTaN/AlCrN multilayer coatings as a function of coating thickness ranging from 1 to more than 20 µm. Various films were prepared by arc evaporation using different substrate types including hard metal, monocrystalline and polycrystalline Al2O3, monocrystalline MgO, and austenite. We found that residual stress peaks in the coatings are relieved by plastic deformation of soft substrate materials. Contrarily, significant residual stresses are built up with increasing coating thickness in the case of stiff substrate types. Additionally, the influence of the multilayer architecture on the residual stress state is discussed. The residual stress state was determined using the sin2Ψ method. Film growth morphology and structure were characterized using cross sectional scanning electron microscopy and X-ray diffraction, and the mechanical properties like hardness and indentation modulus were analysed by nanoindentation.

Authors : V. Dalbauer1, J. Ramm2, S. Kolozsvári3, C.M. Koller1,4, P.H. Mayrhofer1,4
Affiliations : 1Christian Doppler Laboratory for Application Oriented Coating Development, Institute of Materials Science and Technology, TU Wien, Getreidemarkt 9, 1060 Vienna, Austria 2Oerlikon Balzers, Oerlikon Surface Solutions AG, Iramali 18, 9496 Balzers, Liechtenstein 3Plansee Composite Materials GmbH, Siebenbürgerstraße 23, 86983 Lechbruck am See, Germany 4Institute of Materials Science and Technology, TU Wien, Getreidemarkt 9, 1060 Vienna, Austria

Resume : Aluminium oxide is highly valued for many applications due to its exceptional thermo-chemical properties and exhibits – in case of the thermodynamically stable corundum (α) structure – also a high hardness and adequate wear resistance. At deposition temperatures lower than 800 °C, transient oxides, as for instance the γ-Al2O3 phase, are more likely to crystallize during vapour deposition. Even though considerable progress has been made in the last years by the synthesis of (Al,Cr)2O3 solid solutions with corundum-like properties, the deposition of single-phased α-Al2O3 coatings at lower temperatures via physical vapour deposition still poses a great challenge and thus demands further investigations. With the objective to shed further light on the formation of (Al,Cr)2O3, we investigated the structural evolution of intermetallic Al1-xCrx and substoichiometric Al1-xCrxOδ films (with x = 0.1, 0.25, 0.3, 0.50, 0.75), deposited by cathodic arc evaporation, and their oxidation behaviour. The phase composition of our coatings is dominated by Al13Cr2, Al8Cr5, or AlCr2 next to Al and Cr. At low oxygen flow rates during the deposition, the oxide formation proceeds via a distinct refinement of the initially pronounced columnar microstructure. We can show that both, the Al/Cr-ratio as well as the oxygen content of the coatings and their morphology significantly influence the scale formation during post deposition oxidation at temperatures between 900 and 1050 °C.

Authors : Raya EL BEAINOU 1, Nicolas MARTIN 1, Valérie POTIN 2, Paulo PEDROSA 1, Mohammad ARAB POUR YAZDI 1, Alain BILLARD 1
Affiliations : 1 Institut FEMTO-ST, UMR 6174 CNRS, Université Bourgogne Franche-Comté, 15B, Avenue des montboucons 25030 BESANCON Cedex, France 2 Laboratoire ICB, UMR 6303 CNRS, Université Bourgogne Franche-Comté, 9, Avenue Alain Savary, BP 47 870, F-21078 DIJON Cedex, France

Resume : W-Cu thin films were developed using the GLAD co-sputtering technique. The films were produced with two separated W and Cu targets. Both targets were focused on the centre of the substrate and were simultaneously sputtered using opposite and oblique particle incidence angles of 80° from the substrate normal. W and Cu target currents were inversely changed from 50 to 140 mA, so as to tune the elemental concentrations and the microstructure. A shield was added between the W and Cu targets, perpendicularly to the substrate surface, in order to prevent the cross-contamination of the targets. This shield also favors the collimation effect of the W and Cu sputtered particles. Similarly, two argon sputtering pressures were used (0.42 and 1.0 Pa) with and without the shield. The W/Cu weight concentration ratio varied between 0.65 and 20 as a function of the sputtering pressure and target currents. The role of the shield was clearly evidenced and allowed significant variations of the W/Cu ratio. SEM analysis showed a tuneable inclined columnar microstructure. The crystallographic structure (phase occurrence, crystal size) was also influenced by the shield implementation and sputtering pressure. The wide range of DC electrical resistivities (3.6x10-7 to 5.7x10-5 Ohmm) exhibited by these co-sputtered films was discussed considering W and Cu target currents, high and low sputtering pressures and the use or absence of a cross-contamination shield. Keywords: W-Cu films, GLAD co-sputtering, composition, electrical resistivity, microstructure.

Authors : Eon Ju Lee, Ho Young Jun, Si Ok Ryu*
Affiliations : School of Chemical Engineering, Yeungnam University, 280 Daehak-ro, Gyeongsan 712-749, South Korea

Resume : Many industries are recently focused on the development of the inkjet printing technology as well as the appropriate nanoparticle metallic inks for the fabrication of electronic devices. Among conventional metallic inks used in the printing process, silver ink is a typical metallic ink having high conductivity and thermal stability. However, there is a limitation to use it in the fabrication due to its high material cost. Copper is considered as a substitute material for replacing silver, but copper ink has an oxidation issue under atmospheric conditions. Cost effective, highly conductive, and oxidation-free copper nanoparticle ink was synthesized in this study. Copper complexes and copper nanoparticles were used in the synthesis to prevent its oxidation. Expanding its application to various substrates, the synthesized nanoparticles were thermally treated at relatively low temperatures in the range of 200~500℃. The prepared copper ink was printed on the silicon substrate and the printed film was then characterized. Resistivity of the printed electrode was calculated from the cross-sectional area measured by a profilometer and resistance was measured by a digital multimeter. Surface morphology of the prepared electrode was also analyzed using scanning electron microscope (SEM) and atomic force microscope (AFM). From our results, the synthesized copper ink showed the suitable properties to apply to inkjet printing process for the fabrication of various electronic devices.

Authors : Michal Prochazka, Veronika Simova, Jaroslav Vlcek, Radomir Cerstvy, Stanislav Haviar, Jiri Rezek, Karel Rusnak
Affiliations : University of West Bohemia, Univerzitni 8, 306 14 Plzen, Czech Republic

Resume : Thick multilayer (up to 5 layers with a 5 μm thickness each) Zr-B-C, Zr-B-Si-C and Hf-B-Si-C coatings were deposited on silicon and steel substrates using pulsed magnetron co-sputtering of single B4C-Zr(Hf)-(Si) target (at a fixed 15% Zr or Hf fraction and a varying 0-7.5% Si fraction in the target erosion area) in pure argon. A planar unbalanced magnetron (127 × 254 mm2) was driven by a pulsed dc power supply operating at a repetition frequency of 10 kHz with a fixed 85% duty cycle (voltage pulse duration of 85 μs). The total pressure was 0.5 Pa and the substrate temperature was adjusted to 410 °C during the deposition on the substrates at a floating potential. Prior to each deposition of a 5 μm thick layer, a modification of the substrate surface was performed by pulsed dc magnetron sputtering of the B4C-Zr(Hf)-(Si) target in argon at the same pressure of 0.5 Pa, a duty cycle of 20% (voltage pulse duration of 20 μs), a negative dc substrate bias of 1200 V and the substrate temperature of 410 °C for 90-180 min. It was shown that the pretreatment of the steel substrates is a necessary condition for adhesion of the multilayer Zr-B-C, Zr-B-Si-C and Hf-B-Si-C coatings. All coatings possessed a high hardness (up to 32 GPa), high elastic recovery (>70%) and H/E* ratio around 0.1. The 16 μm thick Zr-B-Si-C and Hf-B-Si-C coatings exhibited an enhanced erosion resistance in industrial tests simulating the liquid impact erosion of moving steam-turbine blades.

Authors : Dijo Damien†, Athira Anil†, Dipanwita Chatterjee‡ and Manikoth. M. Shaijumon†
Affiliations : †Indian Institute of Science Education and Research Thiruvananthapuram, Thiruvananthapuram, Kerala, 695016, India. ‡Materials Research Centre, Indian Institute of Science, Bangalore, Karnataka, 560012, India.

Resume : There is an urgent need to develop efficient and cost-effective catalyst for hydrogen evolution reaction (HER) in order to realize a hydrogen economy with clean and renewable energy. Nanostructures of layered transition metal dichalcogenides show promising electrocatalytic activity towards hydrogen evolution reaction, however, majority of the exposed surfaces (basal plane) are inactive, and, engineering their catalytically active edge sites still remains a challenge.[1-2] Here we show that monodisperse single/few-layered MoSe2 nanocrystals can be directly deposited onto any conducting substrate, through electrochemical exfoliation of bulk MoSe2, which exhibit remarkable electrocatalytic activity for the HER with ultra-high efficiency showing very low on-set potential (7 mV vs. RHE) and Tafel slope (31.8 mV dec-1) and good stability after 2000 cycles of CV scans.[3] The exceptional electrocatalytic activity of MoSe2 nanocrystals is resulted from the synergistic advantages emerging from improved edge sites, enhanced electronic conductivity by the presence of co-existing MoO3-x and the presence of new and active sites arising upon in-situ lithiation, all in one step, which is facile, economic and environmentally benign.[4] [1] S. S. Chou, N. Sai, P. Lu, E. N. Coker, S. Liu, K. Artyushkova, T. S. Luk, B. Kaehr, C. J. Brinker, Nat. Commun. 2015, 6. [2] D. Gopalakrishnan, D. Damien, M. M. Shaijumon, ACS Nano 2014, 8, 5297-5303. [3] D. Gopalakrishnan, D. Damien, B. Li, H. Gullappalli, V. K. Pillai, P. M. Ajayan, M. M. Shaijumon, Chem. Commun. 2015, 51, 6293-6296. [4] D. Damien, A. Anil, D. Chatterjee, M. M. Shaijumon, J. Mater. Chem. A (Under revision) 2016

Authors : A. Altaweel, A. Imam, J. Ghanbaja, D. Mangin, P. Miska, T. Gries, T. Belmonte
Affiliations : Université de Lorraine, Institut Jean Lamour, UMR CNRS 7198, Nancy, F-54011, France

Resume : ZnO has gained substantial interest in different research fields due to its attractive properties and wide range of applications. For instance, ZnO is a promising material in photocatalysis applications for water treatment and disinfection. Furthermore, the quantum confinement effect has been widely studied in ZnO nanostructures. The observation of such a phenomenon requires to reach highly crystalline nanostructures with low dimensions. Especially, ultrathin ZnO nanowires have attracted much attention. In this study, the synthesis of ultrathin, single-crystalline zinc oxide nanowires was achieved by treating in a flowing microwave plasma oxidation process zinc films coated beforehand by a sputtered thin buffer layer of copper. The aspect ratio of the nanowires can be controlled by the following experimental parameters: treatment duration, furnace temperature, oxygen concentration. An average diameter of 6 nm correlated with a mean length of 750 nm can be reached with a fairly high surface number density for very short treatments, typically less than 1 minute. The oxidized samples are characterized by means of SEM, XRD, SIMS, HRTEM and EDX techniques. Nanowires are only composed of ZnO without copper particles inside or at the end of the nanowires. Temperature-dependent photoluminescence measurements confirm that ZnO nanowires are of high crystalline quality and thin enough to produce quantum confinement.

Authors : James A. Grant-Jacob, Stephen J. Beecher, David P. Shepherd, Robert W. Eason and Jacob I. Mackenzie
Affiliations : Optoelectronics Research Centre, University of Southampton, Southampton SO17 1BJ, UK

Resume : Pulsed laser deposition (PLD) enables the epitaxial growth of crystalline films using material transfer, from a target to a substrate, via a plasma-plume created during laser ablation. Owing to the several experimental controls available in PLD, which can be adjusted during deposition, this is an excellent tool for growing designer films through altering film parameters such as stoichiometry, crystallinity and thickness [1, 2]. We will present the effects on the refractive index of thin garnet films grown via PLD when varying the temperature of the substrate, onto which the films are grown. Our results show that monotonic control of the YGG refractive index with substrate temperature is possible whilst maintaining good crystal properties. It was observed that at higher substrate temperatures, the gallium content in the crystal is reducing, supported by EDX and XRD measurements, which leads to a decrease in the refractive index of the film. This technique can therefore be used for the fabrication of advanced devices with bespoke refractive index profiles and engineered dielectric properties of composite materials. 1. J. A. Grant-Jacob et al. Opt. Mater. Express 6, 91-96 (2016) 2. T. L. Parsonage et al. Opt. Express 23, 31691-31697 (2015)

Authors : Tomy Acsente, Raluca Florentina Negrea, Leona Cristina Nistor, Elena Matei, Ruxandra Birjega, Christian Grisolia, Gheorghe Dinescu
Affiliations : Tomy Acsente; Ruxandra Birjega; Gheorghe Dinescu - National Institute for Lasers, Plasma and Radiation Physics, Bucharest- Magurele, Romania Raluca Florentina Negrea; Leona Cristina Nistor; Elena Matei - National Institute for Materials Physics, Bucharest- Magurele, Romania Christian Grisolia - CEA, IRFM, Saint-Paul-lez-Durance, France

Resume : Cluster sources based on magnetron sputtering and gas aggregation processes are versatile tools for producing nanoparticles since they allow easy variation of process parameters. In this work, we present results regarding the synthesis of tungsten nanoparticles (WNPs) with very different shapes using a cluster source operated with argon. During the study the working gas pressure and the aggregation length were kept constant while the characteristics of the radiofrequency power applied to the magnetron discharge were modified. Both continuous and rectangular pulsed waves were used: the applied power was 60 W and 100 W in continuous mode while in the pulsed mode the mean power was 60 W (tON = tOFF = 0.2 s). The WNPs were investigated by Electron Microscopy and X-ray Diffraction. The WNPs obtained in continuous mode show a flower-like (60 W) and concave hexapod (100 W) shapes, both presenting dendritic growth. In contrast, the pulsed mode leads to single crystalline cube-octahedral WNPs. All types of WNPs contain both αW (stable) and βW (metastable) phases. The βW phase is dominant in the concave hexapod WNPs and it is remarkable to note the stability of this phase over two years. These results show the ability of this method to produce WNPs with desired shapes for specific applications. Acknowledgements: This work has been financed by the Romanian Ministry of Research and Innvation in the frame of Nucleus programme 4N/2016, and the France-Romania project IFA-CEA C5-07/2016.

Authors : Arnau Oliva Puigdomènech, Jonathan de Roo, José Martins, Zeger Hens
Affiliations : Physics and Chemistry of Nanostructures, Ghent University, Krijgslaan 281-S3, 9000 Gent, Belgium SIM vzw, Technologiepark 935, BE-9052 Zwijnaarde, Belgium Center for Nano and Biophotonics, Ghent University, 9000 Gent, Belgium; Physics and Chemistry of Nanostructures, Ghent University, Krijgslaan 281-S3, 9000 Gent, Belgium Center for Nano and Biophotonics, Ghent University, 9000 Gent, Belgium; NMR and Structural Analysis Unit, Ghent University, Krijgslaan 281-S4bis, 9000 Gent, Belgium; Physics and Chemistry of Nanostructures, Ghent University, Krijgslaan 281-S3, 9000 Gent, Belgium Center for Nano and Biophotonics, Ghent University, 9000 Gent, Belgium;

Resume : Copper nanocrystals (Cu NC) are actively investigated as substitutes for costly silver nanocrystals in conductive inks. However, to be of any use for printed conductors, oxidation of Cu NCs to non-conductive copper oxides must be avoided. Here, we analyze the interplay between the Cu NC surface termination, oxidation suppression and bulk copper formation through thermal annealing using 3 nm Cu NCs synthesized via thermal decomposition of copper formate in oleylamine (OLA). By adapting the method introduced by Sun et al,1 we obtain stable Cu NC dispersions that do not oxidize when stored under inert atmosphere, while showing a rapid conversion into copper oxide when exposed to air or deposited to form a thin NC film. Using solution 1H NMR spectroscopy, we demonstrate that as-synthesized Cu NCs are capped by OLA. OLA is tightly bound at NMR time scales, yet slowly desorbes during storage of the Cu dispersions, a process that is accelerated by oxygen exposure. Addition of carboxylic acids leads to the displacement of OLA from the Cu NCs and the formation of a denser ligand shell, probably consisting of dissociated carboxylic acids. We demonstrate that carboxylic acid ligands make Cu NCs more oxidation proof and facilitate the conversion of films of oxidized Cu NCs into a dense copper film. This offers the prospects of using colloidal Cu NCs as main constituent in conductive, nano-copper inks for applications in printed electronics. (1) Sun, X. et al. Small 2005, 1 (11), 1081?1086.

Authors : Luminita Isac, Ramona Panait, Anca Duta
Affiliations : Transilvania University of Brasov, Centre of Renewable Energy Systems and Recycling, Brasov, Eroilor 29, 500036, Romania

Resume : Even though CuS shows good solar radiation absorbing properties, till now, only few reports were focused on CuS thin films with applications in solar thermal energy conversion. In this work, colored (green) solar selective absorbing coatings Al/Al2O3/CuS were obtained by electrochemical (Al2O3) and spray pyrolysis (CuS) deposition techniques.To improve the coatings’ efficiency, the number of spraying sequences was varied from 5 to 15. Additionally, the effect of a TiO2 anti-reflection and anti-photocorrosion layer on the solar selectivity and stability of the absorbing coating was investigated. The CuS coatings optical properties (solar absorptance, αs, and thermal emittance, εT) were correlated with the chemical composition, crystalline structure and morphology. The results show that samples morphology, homogeneity and porosity (and consequently αs and εT) are significantly influenced by the coatings thickness and density, thus the number of spraying sequences used for CuS film deposition. Solar selective absorbing coatings, with αs ranging from 0.79 to 0.95 and εT = 0.36 - 0.66, were obtained. Durability tests (temperature, UV irradiation and saline aerosols) on the best performing coating, with or without TiO2 layer, evidenced a significant photocorrosion protection and a limited influence on the optical properties. These effects are also depending on the TiO2 layer thickness being recommended a very thin layer which still preserves surface homogeneity.

Authors : A.K. Orlov1, O.O. Zhabynska1, I.A. Vladymyrskyi1, S.M. Voloshko1, S.I. Sidorenko1, K. Kato2, T. Ishikawa2
Affiliations : 1 Metal Physics Department, Igor Sikorsky Kyiv Polytechnic Institute, Ukraine; 2 RIKEN SPring-8 Center, Japan.

Resume : Nanostructured multilayer thin film architectures on the base of FePt system, the influence of heat treatment atmosphere on transformations in [FePt(15 nm)/Au(7,5 nm)/FePt(15 nm)]2x nanothickness multilayer thin films, correlation between nanostructure and functional magnetic and other properties of such nanocomposits were investigated. Films were obtained by magnetron sputtering onto SiO2(100nm)/Si(100) substrates under room temperature and post-annealed at 300°C – 900°C in Ar and Ar + H2 (3 vol.%) atmospheres for 30 s. By synchrotron structural analysis and magnetic properties measurements it was shown that A1-FePt→L10-FePt phase transformation takes place at 500°C irrespective to the heat treatment atmosphere composition. Annealing in Ar atmosphere leads to degree of L10-FePt phase ordering and lattice tetragonal distortion increasing comparing to annealing in Ar + H2 (3 vol.%) atmosphere. Herewith, when hydrogen presences in heat treatment atmosphere this leads to thermal stabilization of L10-FePt grains size (as it was determined by atomic-force microscopy). Heat treatment in Ar + H2 atmosphere leads to post-annealed coercitivity increasing probably due to hydrogen influence on exchange decoupling of FePt grains. Possible models of structure visualization during processes investigated and new trends in thin film materials of such kind are discussed.

Authors : A.K. Orlov1, I.O. Kruhlov1, I.A. Vladymyrskyi1, I.E. Kotenko1, S.M. Voloshko1, S.I. Sidorenko1, K. Kato2, T. Ishikawa2
Affiliations : 1 Metal Physics Department, Igor Sikorsky Kyiv Polytechnic Institute, Ukraine; 2 RIKEN SPring-8 Center, Japan

Resume : Using characterization methods at the nanoscale the correlation between nanostructure of nanothickness V, V/Ag thin films and physical (electrical) properties was investigated. On the basis of these data visualization models of structure and phase composition formation in V(25 nm) and V(25 nm)/Ag(25 nm) thin films during annealing in vacuum 10-3 Pa and 10-7 Pa up to 600°C have been proposed. Films were deposited by PVD electron-beam sequential evaporation in 10-7 Pa vacuum onto SiO2 (001) substrates. According to in-situ electron diffraction characterization the tetragonal distortion of vanadium bcc phase with oxygen solid solution in vanadium (β-phase) formation takes place during films annealing at 400°C in 10-3 Pa vacuum. The vanadium monoxide VO is formed from this phase at temperature of 600°C. Vanadium bcc phase transformation into body-centered tetragonal β-phase within temperature range 400–600°С was analyzed in SPring-8 synchrotron center (beamline BL44B2). The tetragonality is manifested by splitting of (110) vanadium reflection in (101) and (110), (200) reflection – in (002) and (200). The degree of tetragonality depends on annealing temperature and concentrations of O and Ag in V film. The influence of additional Ag layer on nanostructure of V thin films and physical (electrical) properties was studied as well.

Authors : Dima Cheskis
Affiliations : Physics Deartment, Ariel University, Israel

Resume : Unusual electrical and magnetic behaviour of graphene and graphene oxide thin films For more than decade research of graphene and graphene-related materials create a huge interest due to its electronic, optical, magnetic and other properties [1]. Besides interest of fundamental science, graphene and graphene oxide thin films can be part of future electronics devices. It is necessary to develop methods for characterization of electronic and magnetic properties of such thin films. Magnetoresistance measurement is one of such characterization methods. Magnetoresistance, which reflects magnetic dependence of material resistivity, is one of essential effects for manipulating spintronic devices. Magnetoresistance in graphene is usually have very low values in room temperature and low magnetic field. In most experiments magnetoresistance in graphene was shown in the scale of high magnetic field and/or very low temperature [2]. We demonstrate magnetoresistance in room temperature and low magnetic field on mechanically exfoliated bilayer graphene deposited on hexagonal boron nitride. We propose explanation for our results. [1] Geim, Andre K., and Konstantin S. Novoselov. "The rise of graphene." Nature materials 6.3 (2007): 183-191. [2] Gopinadhan, Kalon, et al. "Extremely large magnetoresistance in few-layer graphene/boron-nitride heterostructures." Nature communications 6 (2015)

Authors : Nazar Farid,Gerard M O?Connor
Affiliations : National Centre for Laser Applications (NCLA), School of Physics,National University of Ireland Galway, Ireland

Resume : New technologies are required to precisely structure glass materials. In this paper we present results attained with a polarised short pulse laser to create nanometre periodic structures on the glass. Transparent glass samples of 0.8 mm thickness were initially coated by DC sputtering with Indium tin oxide (ITO) of 175 nm thickness. A laser of 1030 nm wavelength with 10 ps pulse duration operating at 400 kHz was used. A beam scanning system was used to deliver the laser to the coated sample surface using 100 mm focal length lens. For optimal beam shapes and pulse to pulse stability, the laser was operated at maximum power and attenuated using external attenuator. The laser pulse overlap on the ITO film was controlled by adjusting the speed of steering mirrors of galvanometer based beam scanning system and the repetition rate of the laser. The sample was placed on a 3D computer controlled stage which enabled the positon of sample and lens to target distance to be changed with micrometre accuracy. The applied fluence was varied from below the visible damage threshold from 0.4 Jcm-2 of ITO to 1.5 Jcm-2 with multipulses (1 to 30 laser shots per area). At first, periodic nanostructures are generated on ITO films with period 260 nm, corresponding to the forth of incidence laser frequency. With increasing the incident laser fluence or higher SPA, the ITO film is removed and is completely removed at 1.04 J/cm-2 with 25 SPA without effecting or damaging the underlying glass surface. Nanostructures with same period are subsequent generated directly on the glass surface for higher fluences (1.07 Jcm-2) following removal of ITO film. Two type of structures are found, first type with 260 nm period is completed after the forth pulse and is independent of applied fluence. This initial structure evolves to a second structure which is clearly polarisation dependent and starts to grow after the 5th pulse and is firmly established after 12-15 pulses. The ability to structure glass using a laser process offers new opportunities for inexpensive microsystems development.

Authors : Anu Gupta, S.K. Srivastava
Affiliations : Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721302, India ; Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721302, India

Resume : Topological insulators (TIs) have generated a great interest in the fields of condensed matter physics, chemistry and materials science. A topological insulator is a material that is electrically insulating in the bulk, while possessing highly conductive and spin-polarized massless Dirac surface states that are protected against disorder by time-reversal symmetry (TRS), allowing for near dissipation-less transport of spin on the surface [1]. The TRS can be broken by, for example, using elemental doping to induce a magnetic phase in the material. The broken time-reversal symmetry allows for the formation of an energy gap on the surface and is important for many interesting properties in these materials [2]. The second generation 3D TI Bi2Se3 is a class of such materials. To enable a multitude of possible applications of these materials, it is necessary to open a surface energy gap as well as keep the Fermi energy inside the bulk gap [3]. It has been proposed in the literature that doping TIs by magnetic transition metals, such as Fe, Mn, Cr and Co, could break the TRS and open a surface gap [4]. These magnetic impurities also induce electrical doping effect with magnetic effect, i.e., the substitution of Fe 2+ or Co2+ for Bi3+ create hole dopants into the material. On the other hand, when dopants are rare earth metals such as Dy, which are trivalent, only magnetic moments are introduced. The binary compound Bi2Se3 is very popular for TI studies as it has a relatively large bulk bandgap ( ? 0.3 eV) compared with other TIs. One attractive direction in the research is the use of nanostructures, wherein the ratio of surface area to volume is much higher than in bulk materials so that the total conduction from the bulk region is lower, allowing observation of the surface states in certain transport measurements. There is no study performed on rare-earth-metal doped topological insulator nanostructures. In the present study, we synthesized Dy-doped Bi2Se3 nanoplates by a solvothermal reaction. The as-synthesized nanoplates show uniform hexagonal morphology of about 0.16 ?m size and ~ 15 nm thickness. A physical property measurement system (PPMS) is used to determine the temperature dependent magnetization in zero-field cooled and field-cooled cycles between 2 K and 300 K. The doped nanoplates are found to be paramagnetic in the whole temperature range. We also measured the magnetic susceptibility as a function of temperature and found that the effective magnetic moment per Dy is 9.64 ?B, which is close to full moment (10.64 ?B) expected from Hund?s rule. Further experimental and computational studies of electronic and magnetic properties of the system are under way. References: [1] M. Z. Hasan and C. L. Kane, Rev. Mod. Phys. 82, 3045 (2010). [2] J. Wang, X. Chen, B.-F. Zhu, and S.-C. Zhang, Phys. Rev.B 85, 235131 (2012). [3] X. L. Qi, T. L. Hughes, and S. C. Zhang, Phys. Rev. B 78, 195424 (2008). [4] Q. Liu, C. X. Liu, C. Xu, X. L. Qi, and S. C. Zhang, Phys. Rev. Lett. 102, 156603 (2009).

Authors : Manon Gallard[1,2], Mohamed Salah Amara[2], Cristian Mocuta[1], Pierre Noé[3], Chiara Sabbione[3], Françoise Hippert[4], Stéphanie Escoubas[2], Magali Putero[2], Christophe Guichet[2], Marie-Ingrid Richard[2,5], Ariel Brenac[6], Robert Morel[6], Olivier Thomas[2]
Affiliations : [1] Synchrotron SOLEIL, l?Orme des Merisiers, Saint-Aubin?BP 48, 91192 Gif-sur-Yvette, France; [2] Aix-Marseille Université, CNRS, IM2NP UMR 7334, Campus de St-Jérôme, 13397 Marseille, France; [3] Université Grenoble Alpes, CEA-LETI, MINATEC campus, 17 rue des Martyrs, 38054 Grenoble, France; [4] LNCMI, CNRS-UGA-UPS-INSA, 25 rue des Martyrs, 38042 Grenoble, France; [5] ID01/ESRF, The European Synchrotron, 71 rue des Martyrs, 38043 Grenoble, France; [6] CEA/INAC, 17 rue des Martyrs, 38054 Grenoble, France

Resume : Phase-Change materials (PCM) have a great potential for memory device applications in Phase-Change Random Access Memory. The storage mechanism is based on the quick and reversible change in properties between amorphous and crystalline states. X-ray scattering is the adapted tool to investigate in details such a phenomenon. The two states can also be distinguished by following the large contrast in optical reflectivity and electrical resistivity. During the amorphous-crystalline phase transition with temperature, strain and defects accumulation are expected and may contribute to the fatigue of cell memory structure during their functioning (cycling). The possibility of down-scaling PCM requires a better understanding of the phase transition mechanism in order to determine more precisely the relation between strain, surface energy, atomic structure and size as a function of the temperature. The aim of this work is to address the physical phenomena involved during the crystallisation of thin and ultrathin films of chalcogenides. GeTe films (100 down to 5 nm) have been investigated in situ during annealing using coupled i) X-Ray Diffraction, ii) optical curvature and reflectivity measurements, iii) X-Ray Reflectivity, iv) Pair Distribution Function. The experimental approach will be presented and a fine analysis of the amorphous ? crystalline phase transition (in terms of crystallisation temperature, strain, etc.) will be detailed. [work funded by ANR-15-CE24-0021 SESAME project]

Authors : Arsen Hafarov, Ihor Vladymyrskyi
Affiliations : National technical university of Ukraine "Igor Sikorsky Kyiv Polytechnik Institute", Faculty of Physical Engineering

Resume : For several decades, nanoscaled thin-films and coatings played vital roles in modern technologies such as in micro- and nanoelectronics. Moreover, the concept and practice of tailoring the structure and morphology of a given coating or thin film system to modify its properties has been long used to add new functionalities and improved behavior to several materials and devices. Nano-engineering of surfaces is playing a fundamental role in this particular area of research, either in the case of new materials development or in their modification. It is known that even at low temperatures when bulk diffusion processes are practically frozen almost full intermixing of components in thin film heterostructures can occur through grain boundary diffusion and grain boundary diffusion induced motion. In this study, the low-temperature diffusion in Pt/Au/Fe nanolayers was investigated. XRD analysis and SNMS investigation showed that the introduction of an additional intermediate Au layer leads to an enhancement of the low-temperature intermixing of nanocrystalline Fe and Pt thin films. The intermixing at relatively low temperatures is caused by the grain boundary diffusion induced reaction layer formation mechanism. At the same time the ordering is also enhanced, leading to the appearance of the chemically ordered FePt phase, which results in a strongly increased coercivity. At the same time the enhanced chemical ordering is interpreted by stresses developed during the formation of the disordered FePt phase along the grain boundaries: in some of the new grains formed, where there is compressive stress along the {100} directions, chemical ordering can take place.

Authors : G. I. Nkou Bouala 1, A. Etiemble 1,2, C. Der Loughian 1, C. Langlois 1, A. Malchère 1, S. Cardinal 1, J.M. Pelletier 1, J.F. Pierson 2, P. Steyer 1
Affiliations : 1 - MATEIS Laboratory-INSA de Lyon, 21 Avenue Jean Capelle, 69621, Villeurbanne cedex, France 2 - Institut Jean Lamour, Université de Lorraine, 54011 Nancy, France

Resume : Thin film metallic glasses (TFMG) have recently emerged as alternative materials for many applications (micro-electro-mechanical systems and biomedical use), owing to their unique characteristics such as large elastic limit, high toughness and high corrosion resistance. These characteristics are related to their microstructure that lacks long-range-order atomic periodicity and amorphous texture. However, if the mechanical properties of the TFMGs have been largely studied, just few studies have been focused on the understanding of their microstructure evolution during heating. In order to investigate the thermal stability of antibacterial magnetron-sputtered Zr-Cu and Zr-Cu-Ag TFMGs [1], the present study proposes a multiscale characterization involving in situ techniques. First, the crystallization behavior and structural stability were investigated by in situ high temperature XRD combined to DSC experiments, during a continuous heating from room temperature to 600°C under vacuum. Moreover, due to the fast diffusion of silver, silver-based coatings are subject to dewetting. Such process, leading to the formation of micrometric segregated micrometer-sized domains, was observed in situ by using HT-environmental SEM. Finally, at a deeper nanometric scale, in situ HT-TEM was used to observe, during heating, the progressive formation of crystallized grains from the initial amorphous matrix. Through such a multiscale in situ approach, we should better understand the general evolution of the TFMGs under thermal constraint. [1] A. Etiemble et al., Innovative Zr-Cu-Ag thin film metallic glass deposited by PVD magnetron sputtering for antibacterial applications, J. Alloys and Comp. (2016), doi: 10.1016/j.jallcom.2016.12.259.

Authors : Manuela Proença1,2, Joel Borges1,3, Marco S. Rodrigues1, Diogo Costa1,2, Rui P. Domingues1, Paulo Pedrosa4, Nicolas Martin4, Joao P. Dias5, Albano Cavaleiro3, Nenad Bundaleski6, Orlando M.N.D. Teodoro6, Paula Sampaio2, Filipe Vaz1
Affiliations : 1Centro de Física da Universidade do Minho, Campus de Gualtar, Braga, Portugal 2Centro de Biologia Molecular e Ambiental, Universidade do Minho, Campus de Gualtar, Braga, Portugal; 3SEG-CEMUC, Mechanical Engineering Department, University of Coimbra, 3030-788 Coimbra, Portugal; 4Institut FEMTO-ST, UMR 6174 CNRS, Université Bourgogne Franche-Comté, 15B Avenue des Montboucons, 25030 Besançon Cedex, France; 5Instituto Pedro Nunes, Laboratório de Ensaios, Desgaste e Materiais, Rua Pedro Nunes, 3030-199 Coimbra, Portugal; 6Center for Physics and Technological Research, Physics Department, Faculty of Sciences and Technology, Universidade Nova de Lisboa, Campus de Caparica, P2829-516 CAPARICA PORTUGAL.

Resume : The selective detection of flammable and/or toxic gases (e.g. CO), using optical sensors is presently a raising trend over the well-established conductometric-based methods. The present work proposes a reliable and effective possibility of an active material suitable to be used in an optical sensor. It is based on nanocomposite films, containing Au nanoparticles embedded in an oxide matrix. The gas detection mechanism and resolution of the films will be tailored according to the Localized Surface Plasmon Resonance (LSPR) phenomenon revealed by these materials, which is strongly dependent on the composition, distribution, size and clustering tendency of the Au nanoparticles, as well as on the dielectric medium surrounding them. The local changes in the refractive index, such as the ones induced by gas species interacting with superficial nanoparticles, will be used to monitor the LSPR band shifts observed in optimized thin films. Copper oxide (CuO) has been reported to be sensitive to gas molecules, revealing important physical interactions with selected molecules, such as CO. This suggests that it might be an important host for the plasmonic nanoparticles and thus for the detection of gas molecules. In the present work, a set of Au/CuO nanocomposite films were prepared to enable the attainment of gas sensitivity by the tailoring of the nanoparticles growth and coalescence. Preliminary results showed a progressive growth of the Au nanoparticles, together with some crystallization of the dielectric matrix when the annealing temperature was increased. A noticeable nanoplasmonic effect was found for selected thin films and for temperatures higher than 400°C, which will be correlated with their sensing properties.

Authors : Martin Pfaffeneder-Kmen, Günter Trettenhahn, Wolfgang Kautek
Affiliations : University of Vienna, Department of Physical Chemistry, Vienna, Austria

Resume : Graphene oxide (GO) is a potential precursor for graphene. The electrochemical reduction of GO is a potential low-cost and green approach. The cathodic deposition is based on the reduction of GO to reduced graphene oxide (rGO) with reduced solubility accompanied by hydrogen evolution blocking further adsorption of rGO [1,2]. The mechanism of the reduction, as well as the final structure of the reduced form have been the focus of the present study. The reduction of GO was investigated by an spectroelectrochemical in-situ approach. The generation and degeneration of oxygen containing groups and C=C bonds were followed via FTIR spectroscopy. Multivariate Curve Resolution was used to interpret the results. The possibility of controlling the composition and structure of rGO is discussed. [1] M. Pfaffeneder-Kmen, F. Bausch, G. Trettenhahn, W. Kautek, J. Phys. Chem. C 120, 15563?15568 (2016). [2] M. Pfaffeneder-Kmen, G. Trettenhahn, and W. Kautek, J. Phys. Chem. C, 2016, submitted.

Authors : Miroslav Michlíček, Lenka Zajíčková
Affiliations : Miroslav Michlíček Department of Physical Electronics, Faculty of Science, Masaryk University, Kotlářská 2, Brno 61137, Czech Republic Plasma Technologies, CEITEC – Central European Institute of Technology, Masaryk University, Kotlářská, 2, Brno 61137, Czech Republic; Lenka Zajíčková Department of Physical Electronics, Faculty of Science, Masaryk University, Kotlářská 2, Brno 61137, Czech Republic Plasma Technologies, CEITEC – Central European Institute of Technology, Masaryk University, Kotlářská, 2, Brno 61137, Czech Republic;

Resume : Cyclopropylamine, an isomer of widely known allylamine, is a promising candidate for deposition of amine-rich coatings thanks to the low toxicity, excellent stability of prepared coatings and relatively high content of amine groups. However, for further optimization and up-scaling of the process a deeper understanding is crucial. The presented work investigates some fundamental aspects of the deposition process by plasma diagnostics and discusses it within scope of the macroscopic kinetics. The gas phase processes are investigated by mass spectrometry and optical emission spectroscopy, whereas surface processes, mainly the ion bombardment, are studied by retarding field energy analyzer. This work provides insight into the correlation between the inner plasma parameters obtained from diagnostics and properties of the thin film characterized namely by X-ray photoelectron spectroscopy and infrared spectroscopy. Finally, the link between the external parameters and desired thin film properties can be established.

Authors : Vineeta Shukla1,* Suneel Kumar Srivastava2, Sanjeev Kumar Srivastava1
Affiliations : 1Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur-721302, India 2Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur-721302, India

Resume : Abstract: Composition induced quantum phase transition have been found in many alloys. The metallic Pd1-xNix alloy system is one of them. It shows a paramagnetic to ferromagnetic quantum phase transition at a critical concentration xc ~ 0.026 in bulk [1] and in nano dimension [2]. It is well known that when a magnetic impurity couples with conduction electrons, spin-flip scattering known, as the Kondo effect gives rise to an anomalous component of the resistivity at low temperatures. Graphene, a two dimensional structure, is an ideal system to study the Kondo effect owing to its high conductivity. Some experiments suggest that adatoms, vacancies or defects on graphene work as local moments which are usually responsible for its magnetism [3], and sometimes for its the Kondo behaviour [4]. In the present work, we synthesize graphene oxide (GO) by Hummer’s method [5], reduce it to reduce graphene oxide (rGO) using hydrazine hydrate and disperse Pd1-xNix nanoparticles during the synthesis of reduced graphene oxide (Pd1-xNix/rGO) nanocomposites. Chemical reflux method is used to adsorb the Pd1-xNix nano particles on the graphene sheet. After this formation and determination of nanocomposite phase, cystallinity, size and composition has been confirmed by X-ray diffractometer (XRD), X-ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Raman spectroscopy respectively. Magnetic and transport properties of magnetic Pd1-xNix/rGO at low temperature have been measured using physical property measurement system (PPMS). The room temperature M-H plot shows the diamagnetic nature of nanocomposites but, below room temperature, it exhibits the paramagnetic behaviour. On the other hand transport measurements revealed the decreasing nature of resistivity on increasing temperature. Acknowledgement: The work at Department of Physics, IIT Kharagpur was supported by MHRD, India. References [1] Nicklas M., Brando M., Knebel G., Mayr F., Trinkl W., and Loidl A. Phys. Rev. Lett. 82, 4268, (1999). [2] Swain P., Srivastava K. Suneel and Srivastava K. Sanjeev Phys. Rev. B 91, 045401, (2015). [3] Chen, J. H., Cullen W. G., Jang C., Fuhrer M. S. & Williams E. D. Phys. Rev. Lett. 102, 236805 (2009). [4] Chen H. Jian et al., Nature Phys, 1038, 1962, (2011). [5] Kuo D., Chang C., Su T., Wang W., Lin B., Materials Chem. and Phys, 85, 201, (2004).

Authors : Joris More-Chevalier, Ján Lančok, Stanislav Cichoň, Jiří Bulíř, Přemysl Fitl, Vincent Mortet, Petr Ashcheulov, Morgane Poupon, Ladislav Fekete, Gilles Poullain, Christophe Cibert.
Affiliations : Joris More-Chevalier; Ján Lančok; Stanislav Cichoň; Jiří Bulíř; Přemysl Fitl; Vincent Mortet; Petr Ashcheulov; Morgane Poupon; Ladislav Fekete; Institute of Physics of the Czech Academy of Sciences, Prague, Czech Republic Gilles Poullain; Christophe Cibert; Rachid Bouregba; Université de Caen Normandie, ENSICAEN, CNRS UMR 6508 CRISMAT, F-14032 Caen, France.

Resume : The aluminium scandium nitride AlxSc(1-x)N is an interesting material due to a number of potential applications which could be developed in micro electromechanical systems (MEMS). It has been reported that chemical compound influences the physical properties of the mixture, Akiyama et. Al. have observed a maximun piezoelectric response of 27.6 pC/N for a concentration of ~ 40% of Sc in the AlxSc(1-x)N film grown on silicon substrate 1. In this study, we have investigated the crystalline structure, electrical and optical properties of the AlxSc(1-x)N thin films deposited onto MgO and Pt/TiO2/SiO2/Si substrates. Radio frequency magnetron reactive co-sputtering system has been used for films deposition and a large range of concentration has been studied from pure AlN film to pure ScN film. The crystal structure and orientation of the films were investigated by XRD analysis and electrical properties examination was performed with a Physical Property Measurement System (PPMS) and a spectroscopic ellipsometry technique. Also, piezoelectric responses were measured by Piezoresponse Force Microscopy (PFM). The obtained results suggest that AlxSc(x-1)N thin films with a value of x of ~40 % have a high piezoelectric response. This finding is particularly interesting for a development of a magnetoelectric compositie devices where AlxSc(1-x)N thin films might be utilized in piezoelectric components. Acknoweledgments : The work was supported by research infrastructure SAFMAT LM2016088 and by the JoEo Purkyně followship award to V. Mortet. Reference: 1 M. Akiyama, K. Kano, and A. Teshigahara, Appl. Phys. Lett. 95, 162107 (2009).

Authors : S.H. Mousavi, T.S. Müller, P.W. de Oliveira
Affiliations : INM – Leibniz Institute for New Materials, Saarbrücken, Germany

Resume : The conversion or absorber layer is of the most importance for solar cell efficiency therefore controlling its band gap plays an essential role in solar cell industries. In this paper, we present the modification of the band gap of a mixed phase of copper-indium-gallium-diselenide (CuIn1-xGaxSe2) nanoparticles synthesized with a solvothermal method. By increasing the amount of gallium in the structure, the band gap has been increased. Structural and morphological properties of the CIGS nanoparticles were determined by X-ray diffraction spectroscopy, scanning and transmission electron microscopy. Band gap tuning of CIGS thin films could be interesting for optimization of absorber layers in solar cells by enhancing the light absorption from the solar spectrum both in the visible and the ultra-violet range.

Authors : S.A. Camacho1, A.G. Brolo2, R.F. Aroca1,3, C.J.L. Constantino1
Affiliations : 1) Faculdade de Ciências e Tecnologia, UNESP, Presidente Prudente, SP, Brazil 19060-900 2) Department of Chemistry, University of Victoria, Victoria, BC, Canada 3) São Carlos Institute of Physics, USP, São Carlos, SP, Brazil 13566-590

Resume : Surface-enhanced fluorescence (SEF) is observed from molecules located at a certain distance from plasmonic nanostructures that can strongly interact with adjacent fluorophores and it is function of several variables: nanoparticle size and shape, distance between chromophore and nanoparticle, plasmonic surface, and degree of spectral overlap between the chromophore emission and the surface plasmon extinction of nanoparticles. This work reports the use of gold shell-isolated nanoparticles (AuSHINs) to demonstrate an experimental variable for shell-isolated nanoparticle-enhanced fluorescence (SHINEF): tuning the distance between the chromophore and the nanoparticle core by increasing the shell thickness. In previous work we demonstrated that large AuSHINs (Au core size: 100 nm) produce higher enhancement factors (EF) for SHINEF applications than smaller AuSHINs (Au core size: 40 nm), both for 10 nm silica shell thickness. The findings were supported by finite difference time-domain calculations. Now, tuning the thickness of silica shell (0, 4, 7 and 10 nm) surrounding the large AuNPs (core size: 100 nm) allowed achieving different surface-enhanced phenomena, from surface-enhanced Raman scattering (SERS) to SHINEF. AuNPs and AuSHINs were spread onto an Langmuir-Blodgett monolayer of zinc(II)-protoporphyrin(IX) dimethyl ester resulting in SERS EF ~ 103 for AuNPs and SHINEF EF = 18, 23 and 29 for AuSHINs with 4, 7 and 10 nm of silica thicknesses, respectively.

Authors : S.R. Pratas (1), A.V. Girão (1), M.A. Neto (1), E. Soares (2), R.F. Silva (1), F.J. Oliveira (1)
Affiliations : (1) Department of Materials and Ceramic Engineering, CICECO, University of Aveiro, 3810-193 Aveiro, Portugal; (2) DURIT - Metalurgia Portuguesa do Tungsténio, Lda. Arruamento C, 3854-909 Albergaria-a-Velha, Portugal

Resume : The deposition of diamond films on hardmetal (WC-Co) substrates requires prior preparation of the substrate in order to passivate cobalt and thus prevent the formation of sp2 C-bonds instead of sp3. This formation of graphite compromises the mechanical properties of the interface between the diamond film and the substrate, causing lack of adhesion of the coating. Several methods are used to remove cobalt or hinder its surface segregation, such as acid pretreatments or metallic carbide interlayers between the substrate and the diamond film. In this work we developed in-situ tungsten/titanium carbide interlayers and compared them with a commonly used acid pretreatment (Murakami followed by H2SO4/H2O2) on hardmetal. This is a new, environmentally friendly, one-step approach, allowed by the flexibility of HFCVD reactors, that precludes the use of acids and ensures the high adhesion required by machining operations. The effect of the substrate temperature cycle on adhesion, growth rate and micro- and nanocrystalline diamond quality was also studied using drill bits and end mills tools as substrates. The diamond film adhesion was measured by indentation tests on square hardmetal plates and by drilling tests on MMC parts. The development was closely followed in every step with a characterization of the coated sample by µ-Raman spectroscopy and scanning electron microscopy.

Authors : Thi Kim Hang Pham1, Nyun Jong Lee1, Ki Hoon Kang2, Eun Sang Park3, Anny Michel4, Tae Hee Kim1*
Affiliations : 1Department of Physics, Ewha Womans University, Seoul 120-750, Republic of Korea; 2 Department of Materials Science and Engineering, Hanyang University, Seoul 133-791, Republic of Korea; 3KU-KIST Graduate School of Converging Science and Technology, Korea University, Republic of Korea;4Départment de Physique et Mécanique des Matériaux, CNRS-Université de Poitiers-ENSMA, France

Resume : In view of fact that the pure spin Hall magnetoresistance (SMR) effect was only observed in nonmagnetic metal (NM)/ ferromagnetic (FM) insulator systems such as YIG/Pt and Pt/CoFe2O4, a FM insulator-based hybrid structures came in to focus [1]. Much attention has been given to the SMR phenomena in NM/FM oxide structures due to their applicability to the control of the magnetization direction via the in-plane current. Here, we report the anomalous Hall resistance and the anisotropic magnetoresistance (AMR) of Pt bars deposited on Fe3O4/MgO/Ta multilayer stacks on top of unetched Si substrates. The temperature dependence of the AMR in a set of Pt/Fe3O4/MgO/Ta hybrid structures was explored as a function of Pt thickness ranging from 2.0 and 4.0 nm and Fe3O4 thickness ranging from 2.0 and 40.0 nm. In order to determine the spin mixing conductance at the Pt/Fe3O4 interface, magnetization orientation dependent magnetoresistance (MR) was carefully analyzed. The AMR was obtained ~ 0.1 % at 100K below the Verwey transition temperature for a 2.0-nm-thick Pt film grown on a 40-nm-thick Fe3O4 film, in which a much higher MR ratio was seen than samples with thicker Pt thickness. However, the Fe3O4 thickness dependence of the AMR did not clearly reveal. Intriguingly, the spin mixing conductance at the interface is found to be different depending on the structural and electrical properties of Fe3O4 thin films. Therefore, the effect of the roughness and crystallinity of the Fe3O4 films on the AMR behavior were also investigated as well. [1] M. Weiler, M. Althammer, F. D. Czeschka, H. Huebl, M. S. Wagner, M. Opel, I. Imort, G. Reiss, A. Thomas, R. Gross, and S. T. B. Goennenwein, Physical Review Letters 108, 106602 (2012)

Authors : I.Saafi1, G. Schmerber2, A. Amlouk1, A.Dinia2, M. Amlouk1
Affiliations : 1 Unité de Physique des dispositifs à Semi-conducteurs UPDS, Faculté des Sciences de Tunis, Université de Tunis El Manar, Tunisie. 2 Université de Strasbourg, CNRS, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), UMR 7504, 23 rue du Lœss, B.P. 43, 67034 Strasbourg Cedex 2, France

Resume : The development of transparent conducting coatings as thin film-electrodes with interesting physico-chemical characteristics like high electron work function, high electron mobility and high transparency, hence, is becoming more relevant. Indeed, to meet these forthcoming requirements, novel alloys or cost-effective preparing techniques are in demand. One of these approaches is focusing on a preparation of ternary oxides by the spray pyrolysis technique. This work deals with some physical studies on SnO2–ZnSnO (TO-ZTO) alloy sprayed nanofilms grown on sapphire substrates at different temperatures (450°C and 600°C). The structural and optical properties were investigated using X-Ray diffraction (XRD), UV visible spectroscopy and Photoluminescence (PL) techniques. XRD results reveal the existence of a mixture of SnO2/ZnSnO3 and SnO2/Zn2SnO4 phases at T=450°C and 600°C, respectively. The structural analysis shows that both phases are polycrystallines. On the other hand, the optical constants (refractive index, extinction coefficient and the dielectric constants) have been obtained by the transmittance and the reflectance data. The optical band gap energy value changed from 3.96 eVdown to 3.78 eV as substrate temperature increased from 450°C up to 600°C. The room temperature photoluminescence results reinforce this finding regarding the existence of three phases (SnO2, ZnSnO3 and Zn2SnO4) which is consistent with X-Ray diffraction analysis.

Authors : P. Dub?ek, B. Pivac, N. Radi?, N. Krstulovi?, M. Bi??an and S. Bernstorff
Affiliations : Rudjer Boskovic Institute, Bijenicka 54, HR-10000 Zagreb, Croatia; Institute for Physics, Bijenicka 46, HR-10000 Zagreb, Croatia; Elettra-Sincrotrone Trieste, SS 14, km 163.5, Basovizza (TS), Italy

Resume : Plasmonic nanoparticles doping of solar cells improves power conversion efficiency. It is believed that it will be implemented in 4th generation solar cells. The metallic nanoparticles must be incorporated into the cell production, and this limits available annealing temperature range, since the cell is temperature sensitive itself. This leads to compromises in size and shape distribution widths of the plasmonic nanoparticles. Pulsed laser annealing is proposed as a solution: it is limited to the metallic film on top, and the energy for the deweting is supplied to it, leaving the structure below virtually unchanged, regardless the number of applied pulses. Here we report the study of laser annealed aluminium nanoparticle production. Magnetron sputtering at room temperature was employed in production of smooth Al films on monocrystalline silicon. The thickness of films was 10 nm. The films have been annealed by pulsed infra red laser. Pulse energy fluence was varied from 70 to 200mJ/cm2, and the number of pulses from 1000 to 10 000. The size distribution and uniformity of irradiated surface was invrstigated using AFM and GISAXS. The initial film was already nanostructured: its surface is one of densily packed nanopfeatures that are 1.6 nm high. After annealing with 5000 pulses of 120mJ/cm2 energy fluence, larger particles of irregular shape are grown, but they are surrounded by remnants of initial rough surface features. An even distribution of particles was produced when the number of pulses was increased to 10000. Lateral size distribution is significantly sharpened, while the height distribution remains relatively wide. A bimodal particle distribution was produced when th fluence was 150mJ/cm2. Generally, increment of fluence resulted in increased particles height, while the lateral dimensions did not change significantly.

Authors : Ah Ram Kwon, Dong Won Han
Affiliations : Korea Institute of Industrial Technology

Resume : Due to the high saturation magnetization and coercivity, permanent magnet with rare-earth components have been used in the industrial applications such as not only mechanical parts but also electrical and electronic products. However, rare-earth components have strong dependency on rare-earth elements limited and regionally concentrated supply. To overcome this problem, investigation of rare-earth free magnets are necessary. In this study, among rare-earth free magnetic materials, Fe16N2 films shown significantly high saturation magnetization on several previous papers were deposited on Si (001) by RF magnetron sputtering. A ratio of Fe16N2 in the Fe-N film affects saturation magnetization. However, even though film deposited with optimum deposition conditions (partial pressure of gases, power etc), films show different properties depending on thickness of the films. In this work, we investigated relation between magnetic properties and thickness. Crystallization and the ratio of Fe16N2 in the Fe-N film were measured by X-Ray Diffraction (XRD) and X-Ray Photoelectron Spectroscopy (XPS). Magnetic properties were measured by Vibrating Sample Magnetometer (VSM). Surface morphology and a structure were shown with Field Emission Scanning Electron Microscope (FE-SEM).

Authors : V. Siropoulos, D. Chaliampalias, D. Karfaridis, C. Vogiatzis, P. Patsalas, S. Skolianos, M. Stefanidou, E. Pavlidou, G. Vourlias
Affiliations : Aristotle University of Thessaloniki

Resume : The problem of structural steel corrosion occurs to a great extent, due to the increasing use in any kind of construction, while it worsens in areas with highly corrosive environments such as seaside and heavy snowfall regions due to the intense presence of Cl- ions. For the protection of structural steel hot-dip galvanizing is the most common coating technique and widely applied in industrial scale. The protection mechanism is based on the cathodic protection of the ferrous substrate from Zn and consists in converting the substrate in cathode of a galvanic element. The result is that oxidation reactions do not occur on the metal substrate, and thus it is protected. However, the protection potential of these coatings is significantly reduced in areas with high chloride concentration. In the present work the deposition of hot dip Zn coatings reinforced with oxide compounds is investigated. The specimens were dipped into a bath containing Zn, Al and metal oxide nanoparticles (Al2O3, TiO2, SiO2), in order to create oxide inclusions in the body of the coating, which act as a barrier against the diffusion of chlorides. The whole deposition setup was in a controlled Ar purged atmosphere in order to prevent the reaction of the molten metal bath with oxygen. The experimental data were acquired from Scanning Electron Microscopy (SEM) and X-Ray analysis (XRD). Furthermore an assessment of the corrosion resistance was made by electrochemical corrosion measurements.

Authors : Ines Lachebi, Abdelkrim Fedala, and Mohamed Kechouane
Affiliations : USTHB, Faculté de Physique, Laboratoire de physique des matériaux, Equipe Couches Minces et Semiconducteurs, B.P. 32, El Alia, 16111 Bab-ezzouar, Algers, ALGERIA

Resume : Aluminum nanoparticles are deposited by the thermal evaporation method. During deposition the substrates are heated and maintained at fixed temperature (200-580°C). The used substrates are corning glass and crystalline silicon wafer oriented (100). Two series of samples are deposited one by varying the deposition temperature and the other the deposition time. The deposition is occurred at residual pressure less than 10-5 mbar. The evaporated aluminum rate is the same at each deposition thus the deposition time determine the deposited aluminum amount. The samples are characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and optical transmission in the uv-vis-ir range. The morphological parameters as nanoparticles size, density, and circularity are extracted using ImageJ program software. For all samples the SEM images show two kind of nanoparticles small and large with size around 10-20 nm and 60-150, respectively. The determined morphological parameters show coherent evolutions with the variation of the temperature of substrates and deposition time.

Authors : C. I. da Silva Oliveira 1, D. Martínez-Martínez 1, L. Cunha 1, E. Alves 2, N. P. Barradas 3 M. Apreutesei 4
Affiliations : 1 Center of Physics, University of Minho, Campus de Azurém, 4800-058 Guimarães, Portugal; 2 Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela LRS, Portugal; 3 Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela LRS, Portugal; 4 INSA de Lyon, MATEIS Laboratory, Villeurbanne, France

Resume : Zirconium oxynitride coatings are an interesting choice for aesthetic purposes, due to the combination of chemical stability, biocompatibility, good mechanical properties and a nice palette of colors achievable. Additionally, its preparation by reactive magnetron sputtering is relatively easy and simple. However, the chemical composition of films lays in a very particular region of the Zr-O-N ternary diagram, which is probably one the main reasons behind the limited palette of the observed colors. In this contribution, we will make a complete study of the Zr-O-N system, including an exhaustive comparison with literature. First, the deposition parameter space is explored, by changing target power, bias and composition of the sputtering atmosphere. The inclusion of Ti as dopant has been explored as well. The chemical and phase composition and structure of the films are evaluated by RBS, XRD and SEM, respectively, and correlated with the synthesis conditions. Finally, the color of the coatings is measured by spectrophotometry and interpreted in terms of the characteristics of the films.

Authors : M. Novotny1, P. Dusek1, J. Nikl2, J. Bulir1, P. Pokorny1, E. Maresova1, P. Fitl3, L. Fekete1, J., Y. Dekhtyar4, J. Lancok1
Affiliations : 1) Institute of Physics of the Czech Academy of Sciences, Na Slovance 2, 182 21 Prague, Czech Republic; 2) Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, V Holesovickach 2, 180 00 Prague 8, Czech Republic; 3) University of Chemistry and Technology Prague, Technicka 5, 166 28 Prague 6, Czech Republic; 4) Riga Technical University, 1 Kalku str., Riga, Latvia

Resume : Black aluminium thin films were prepared by means of pulsed DC magnetron sputtering. The films were deposited from pure aluminium target and their properties modification is reached by proper variation of deposition conditions, such as adding nitrogen to argon working gas of partial pressure from 0.5·10-3 Pa to 2·10-2 Pa. Black aluminium (it could be also referred as aluminium blacks) thin films exhibit, due to specific surface micro-nanostructure, excellent absorptivity in UV-VIS-IR electromagnetic radiation spectral regions. The film properties were examined by spectrophotometry, AFM, SEM, photoelectron spectroscopy. The deposition method allows effective, low cost fabrication of coatings on several kinds of substrates (eg. glass, stainless steel) and it is also suitable for large area substrates coating. Noble metal coating of black aluminum layer can be used toward further improvements on the properties mentioned above and to serve as its protection. The coating could find other application as absorbers of electromagnetic radiation, plasmonics, detectors, chemical sensors.

Authors : Tahir Ahmad, M, Kamran, M. U. Manzoor, M. T. Z. Butt
Affiliations : Department of Metallurgy and Materials Engineering, CEET, University of the Punjab Lahore Pakistan

Resume : The intumescent coatings are passive fire protection of materials widely used for steel protection. The intumescent and subsequent char formation process helps to keep the steel temperature below its limiting temperature and to provide the fire-resistance. Our current research is based on studying the effects of adding silica sand nano-particles on epoxy based intumescent coatings. The effect of variation of 2,4, 6 and 8wt.% of silica sand nano-particles are blended in epoxy resins with fixed amount of hardeners. The prepared paste is deposited on mild steel grade 1020 by manual process. The prepared coatings are burned from four different corners to analyze the char microstructures with scanning electron microscope (SEM) with the help of EDX. The results showed the rapture surfaces and presence of holes, clusters and porous surface are due to the inappropriate mixing of silica sand nano-particles in char microstructures. The hardness of coating are determines that how much the coating withstand at specific force. The themo gravimetric analysis tells us about the weight loss percentage by increasing the temperature range; it also gives us information about thermal stability factors.

Authors : O. Yastrubchak, L. Gluba, M. Sawicki, T. Andrearczyk, J.Z. Domaga?a, J. ?uk, T. Wosinski, J. Sadowski, N. Tataryn
Affiliations : V.E. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine, 03028 Kyiv, Pr. Nauky 41, Ukraine; Institute of Agrophysics, Polish Academy of Sciences, Do?wiadczalna 4, 20-290 Lublin, Poland, Institute of Physics, Maria Curie-Sklodowska University in Lublin, Pl. M. Curie-Sk?odowskiej 1, 20-031 Lublin, Poland; Institute of Physics, Polish Academy of Sciences, Al. Lotnikow 32/46, 02-668 Warsaw, Poland; Institute of Physics, Polish Academy of Sciences, Al. Lotnikow 32/46, 02-668 Warsaw, Poland; Institute of Physics, Polish Academy of Sciences, Al. Lotnikow 32/46, 02-668 Warsaw, Poland; Maria Curie-Sklodowska University in Lublin, Pl. M. Curie-Sk?odowskiej 1, 20-031 Lublin, Poland; Institute of Physics, Polish Academy of Sciences, Al. Lotnikow 32/46, 02-668 Warsaw, Poland; MAX-IV laboratory, Lund University, P.O. Box.118, 22100 Lund, Sweden, Department of Physics and Electrical Engineering, Linnaeus University, SE-391 82 Kalmar, Sweden, Institute of Physics, Polish Academy of Sciences, Al. Lotnikow 32/46, 02-668 Warsaw, Poland; Kyiv Technical University, 37, Prosp.Peremohy, 03056 Kyiv, Ukraine;

Resume : The GaAs based ferromagnetic semiconductor alloy compound containing Mn, Bi and In emerged as potential candidates for novel microelectronic and spintronic application. The (Ga,Mn)As has become a model diluted p-type ferromagnetic semiconductor, in which a few percent of Ga lattice atoms have been substituted by Mn atoms. All the epitaxial layers with the thicknesses up to 100 nm were grown using low temperature (230_C) MBE pseudomorphically on semi-insulating (001) GaAs and InGaAs substrates. The alloy compositions were determined using high resolution X-ray diffractometry (XRD) followed by the in-situ Reflection High Energy Electron Diffraction (RHEED). The quality of the epi-layers were estimated using transmission electron microscopy (TEM). The superconducting quantum interference device (SQUID) magnetometry have been used for the investigation of the magnetic properties of the heterostructures. Photoreflectance (PR) measurements were used the determination of the band gap (E0) and spin-orbit split-off (E_SO) band to conduction band optical transitions. The results presented in the our last publications concerning the ferromagnetic (Ga,Mn)As and bismuth doped (Ga,Mn)As, have shown the merit of the use the PR method for the band structure analysis of the GaAs base epitaxial layers. Besides the PR technique, the samples have been investigated by the ?Raman spectroscopy to confirm p-type character of some films by the observation of the Coupled Plasmon-LO Phonon Mode (CPPM). The in-situ UV Angle Resolved Photoemission Spectroscopy (ARPES) was used for the band structure analysis of the epitaxial layers.

Authors : O. Dikaya (a), A. Goikhman (a), D. Novikov (b), E. Mukhamedzhanov (c), M. Borisov (c), K. Maksimova (a)
Affiliations : (a) Immanuel Kant Federal Baltic University, Kaliningrad, Russia; (b) Deutsches Elektronen-Synchrotron (DESY), Hamburg, Germany; (c) National Research Center "Kurchatov Institute", Moscow, Russia

Resume : Recently multilayer structures (MS) have found a wide range of applications, and one of the most specific of them is the X-ray standing wave (XSW) research technique for localization chemical elements in molecular layers [1]. The MS quality should be very high to meet all the requirements of application: few nanometers (1-10 nm) of individual uniform layer thickness, angstrom-smooth interfaces and number of layers up to several hundred. Additionally, the MS materials shouldn?t have secondary x-ray fluorescence in the region of interest. In this work, we report about Al/Ni and AlOx/NiOx MS fabricated by Ion Beam Deposition method using Ar and Kr plasma. All samples had 20 periods with thickness around 6.2 nm. The MS were studied by atomic force microscopy and X-ray reflectivity laboratory technique. The following structural parameters were achieved: surface roughness 0.4 nm for Al/Ni and 0.2 nm for AlOx/NiOx, as well as interdiffusion thickness 0.7 nm for Al/Ni and 0.25 nm for AlOx/NiOx. X-ray reflectivity of the first Bragg peak is 50% for Al/Ni and 43% for AlOx/NiOx at 8.048 keV (Cu K-alpha). The XSW experiment was done on Kurchatov Specialized Synchrotron Radiation Source (Phase beamline) in Moscow to compare XSW generation capabilities of structures. [1] E. Schneck, et. al., Proceedings of the National Academy of Sciences of the United States of America 9521-9526 (2016) 113

Authors : A. Tlili1, 2, S. Pailhès1, R. Debord1, S. Gravier2 ,J.- J. Blandin2, P. Noé3. V. M. Giordano1
Affiliations : 1 Institute of Light and Matter, UMR5306 Université Lyon 1-CNRS, Université de Lyon, 69622 Villeurbanne Cedex, France” 2 Science and Engineering of Materials and Processes, SIMaP, GrenobleINP, 38402 Saint-Martin d’Hères, France 3 CEA- LETI, Minatec Campus, 38054 Grenoble Cedex 09, France

Resume : One of the most important challenges of our society consists in solving the thermal management problem, which strongly limits any further development in technologies such as data storage and energy harvesting. At this day, nanostructuration is one of the most successful strategies for reducing thermal conductivity: its success can be intuitively understood in terms of an enhanced phonons scattering from grain borders, which reduces their mean free path down to the one typical for a topologically disordered structure, resulting thus in a very low thermal conductivity. In order to get a better insight into the microscopic mechanisms behind the thermal conductivity reduction due to nanostructuration, we have investigated the phonon dynamics in two materials whose nano-crystalline and amorphous phases are of high technological interest: a Zr-based multi-component metallic alloy renowned for its excellent mechanical properties, and a doped GeTe thin film used as phase change memory material. By means of X-ray inelastic scattering we have been able to measure the acoustic phonons both in the nanostructured and amorphous phase, thus getting a microscopic understanding of the effects of nanostructuration on phonons, compared with the effect of the topological disorder.

Authors : F. Pappa, V. Karagkiozaki, Z. Dardani, P. Gkertsiou, S. Kassavetis, C. Gravalidis, S. Logothetidis
Affiliations : Nanomedicine Group, Lab for Thin Films-Nanobiomaterials-Nanosystems & Nanometrology (LTFN), Department of Physics, Aristotle University of Thessaloniki, Greece

Resume : Despite multiple research approaches to prevent bacterial colonization on surfaces, infections are still a major problem with high health care costs respectively. Antibacterial activity of zinc oxide nanoparticles (ZnO-NPs) has received significant interest worldwide, since they can enhance the successful implementation as advanced antibacterial surface coatings. ZnO-NPs exhibit attractive antibacterial properties due to increased specific surface area as the reduced particle size leading to enhanced particle surface reactivity. It is proposed that both the abrasiveness and the surface oxygen species of ZnO nanoparticles promote the biocidal properties of ZnO. In this current work ZnO nanoparticles were prepared by two precipitation methods using zinc acetate dehydrate (Zn(CH3COO)22H2O), sodium hydroxide (NaOH) and polyvinylpyrrolidone (PVP) as a surfactant in the first one and zinc nitrate (Zn(NO3)2¬) and sodium hydroxide (NaOH) in the second. The engineered nanoparticles were characterized by Atomic Force Microscopy (AFM), x-ray diffraction (XRD) analysis and Transmission Electron Microscopy (TEM) to decide the differences between the NPs of the two different methods concerning the size distribution, the shape and the morphology of the particles. AFM revealed at both samples a unique nanoparticulate morphology, with average size diameter 60nm. The presence of ZnO was established via XRD measurements and TEM imaging provided a valuable tool for the nanoparticles’ morphology. After the successful fabrication of both methods, AFM revealed that the optimum morphology and size distribution of the fabricated nanoparticles were at the second one. TEM imaging further reinforced those results, via the morphology analysis. The nanoparticles were incorporated into polymer mats and matrices and the properties of these surfaces with or without the presence of nanoparticles were investigated via Nanoindentation measurements. The NPs from both methods are very promising alternatives as antimicrobial agents for antimicrobial surfaces. Acknowledgements: This work has been partially supported by the NANOCARDIO Project “Nanomedicine for Advanced Bioactive/mimetic materials for Cardiovascular Implants” and by NanoReg II

Authors : B.O. Postolnyi1,2, G. Abadias3, L. Rebouta4, J.P. Araujo2, A.D. Pogrebnjak1
Affiliations : 1Sumy State University, 2 Rymskogo-Korsakova st., 40007 Sumy, Ukraine 2IFIMUP and IN-Institute of Nanoscience and Nanotechnology, Department of Physics and Astronomy, Faculty of Science, University of Porto, 687 Campo Alegre st., 4169-007 Porto, Portugal 3Institut Pprime, Department of Physics and Mechanics of Materials, CNRS - University of Poitiers - ENSMA, 11 Blvd. M. et P. Curie, BP 30179, F86962, Chasseneuil-Futuroscope cedex, France 4Centre of Physics, University of Minho, Alameda da Universidade, 4804-533 Guimarães, Portugal

Resume : Multicomponent multilayer TiAlN/SiAlN thin films were deposited in Nitrogen and Argon atmosphere by magnetron sputtering from two TiAl and SiAl targets on set of various substrates: glass, silicon, high speed steel. Total coatings thickness varies in range 0.1÷1.5 µm and individual layer is expected to be from 4 to 20 nm. Basic morphological and elemental analysis was performed using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). As advanced non-destructive analysis, various method of X-ray diffraction (XRD) were used. Calculation of bilayer thickness in thin films deposited of silicon substrates and evaluation of roughness were done using data of X-ray reflectivity (XRR) analysis. Results of measurements were also crosschecked with values obtained by SEM on cross-section samples. Initial phase identification was performed with conventional θ/2θ XRD patterns. To control X-ray beam penetration depth and to obtain information about phase evolution through the films depth profile the grazing incidence and in-plane XRD scanning were used. Appropriate lattice parameters, as well as crystalline size, were calculated. Residual stresses were evaluated from d-spacing vs sin2ψ plots. Considered techniques have demonstrated their advantages in analysis of multilayer samples.

Authors : Malgorzata Holynska, Ricardo Martins, Adrian Graham, Yuriy Butenko, Frank Meyer, Christopher Semprimoschnig
Affiliations : European Space Agency, Keplerlaan 1, NL2200AG, Noordwijk; European Space Agency, Keplerlaan 1, NL2200AG, Noordwijk; European Space Agency, Keplerlaan 1, NL2200AG, Noordwijk; European Space Agency, Keplerlaan 1, NL2200AG, Noordwijk; CeraNovis GmbH, Untertuerkheimer Strasse 25, 66117 Saarbruecken; European Space Agency, Keplerlaan 1, NL2200AG, Noordwijk

Resume : BepiColombo is a mission planned by the European Space Agency (ESA) to reach Mercury, the least explored planet in our Solar System. The mission will face long-term exposure to high temperatures up to 350 deg. C, thermal cycling between extreme temperature values, and high levels of radiation. A new porous “Nanovation” coating (V14) was developed by Ceranovis in cooperation with ESA to deal with the harsh conditions. The coating comprises a sintered mixture of oxides/nitrides using a silicate binder deposited on a titanium substrate. Results of tests conducted by ESA will be presented. The coating’s structural integrity was followed using PXRD. Impact of sealing of the a priori porous coating with additional agents, batch variability, environmental testing and in situ thermal cycling were assessed.

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Hard, wear self-healing, self-lubricant and corrosion/oxidation resistant coatings : Ph. Steyer + Diego Martinez
Authors : Peter Panjan
Affiliations : Jozef Stefan Institute, Jamova 39, 1000 Ljubljana, Slovenia

Resume : All imperfections on the surface of coated tools have a strong influence on their tribological performance. In the running-in phase, the real sliding contact area is limited to the asperities, which tend to be cut off or fractured due to mechanical loading. The most common asperities on coated tools are nodular defects. During the operation of tools, different failures of tool's surface can be caused by cracks that initiate at coating defects. Particular problem are nodular defects, which collapse and form abrasive particles in the sliding contact area. High shear stresses cracks are also induced in the coating matrix. For these reasons the abrasive wear is very intensive during the run-in period. An imperfection on the surface of forming tool also represents a potential initial point for the beginning of galling and sticking of the workpiece material. All PVD hard coatings also contain some degree of microporosity; i.e., open pores, pinholes, void zones around the nodular defects or droplets, microcracks and pores between the columns. Such coating imperfections significantly reduce its protective nature in a corrosive media. In this work the processes that occur between the coating containing defetcs and a typical tribological counter body (Al2O3and 100Cr6) are analyzed. We will present the role of growth defects in the sputter deposited TiAlN coating during the running-in period of the ball-on-disk tests.

Authors : Matthieu Lagarde, Niusha Shakibi Nia, Juan Creus, Xavier Feaugas, Alain Billard, Catherine Savall
Affiliations : Matthieu Lagarde, Juan Creus, Xavier Feaugas, Catherine Savall: LaSIE, Université de la Rochelle, UMR 7356 CNRS, Av. Michel Crépeau, 17042 La Rochelle, France; Niusha Shakibi Nia: Institut für Physikalische Chemie, Leopold-Franzens-Universität Innsbruck, Innrain 52c, 6020 Innsbruck, Austria; Alain Billard: IRTES-LERMPS, UTBM Montbeliard, 2 place Tharradin, 25200 Montbéliard, France;

Resume : Among the candidates for the substitution of hard chromium, Ni-W alloys present attractive mechanical and tribological properties. These alloys are often obtained by electrodeposition, but nickel salts are harmful species for the environment and for the health. Magnetron sputtering could be an alternative method to deposit these alloys. Thus, the aim of this study is to compare the properties of Ni-W coatings deposited from both methods and particularly their corrosion resistance. The W content varied between 0 and 18 at.% for the electrodeposits and from pure Ni to pure W for the PVD coatings. Polarization curves and electrochemical impedance spectroscopy measurements were performed in acidic sulfuric solutions. Even if the same trend is followed regarding the influence of W, PVD coatings show a higher reactivity than electrodeposited coatings. A careful control of the metallurgical states of the coatings was performed to explain this behavior. The microstructure and the contamination of the coatings were characterized by using different techniques in order to evaluate grain size, crystallographic texture, nature of grain boundaries, morphological defects, impurities contents…The nature of the corrosion products was also investigated by using Raman and XPS spectroscopy. Results were then compared for both processing techniques in order to identify which metallurgical parameters are responsible for the higher reactivity of the PVD coatings in acidic solutions.

Authors : Imane Bouabibsa, Salim Lamri, Frédéric Sanchette
Affiliations : Institut Charles Delaunay, Laboratoire des Systèmes Mécaniques et d’Ingénierie Simultanée (ICD-LASMIS) UMR 6281, CNRS-UTT, Antenne de Nogent-52, Pôle Technologique de Haute-Champagne, 52800 Nogent, France. Nogent International Center for CVD Innovation (NICCI), LRC CEA-ICD LASMIS, UTT Antenne de Nogent, pôle technologique de haute Champagne, 52800 Nogent, France

Resume : Diamond-like carbon (DLC) coatings have been widely used in many mechanical applications and attracted significant attention owing to their excellent properties including high hardness, low friction coefficient and high wear-resistance. This work presents a study of The influence of pure Ti, Nb or Cr adhesion interlayers on the tribological properties and impact wear resistance of Diamond like carbon (DLC) coatings deposited on high speed steel (M2) substrates using hybrid deposition process that combines radio frequency plasma enhanced chemical vapor deposition (RF PECVD) and magnetron sputtering in Ar, H2 and C2H2 gas mixture atmospheres. Impact-wear tests were used to study the interface deformation, contact failure and wear mechanisms. A 6 mm diameter steel 100Cr6 ball was used as the impacting body and the impact frequency was set at 10 Hz. After these tests, the wear craters were studied by 3D microscope, and non-contact profilometer. The structure was investigated by scanning electron microscopy. Chemical bonding was studied by Raman spectroscopy and X-ray photoelectron spectroscopy. The friction and wear behaviors were characterized using a ball-on-disk tribometer. Mechanical properties including residual stress, hardness, adhesion strength were evaluated by nanoindenter, scratch tester and surface profiler.

Authors : Federico Veronesi1, Mariarosa Raimondo1, Giulio Boveri1, Claudia Nicolai2, Elena Ciappi2, Francesco La Gala2
Affiliations : 1CNR-ISTEC, Institute of Science and Technology for Ceramics, National Research Council, Faenza (RA), Italy; 2 CNR-INSEAN, Marine Technology Research Institute, National Research Council, Rome, Italy

Resume : Superhydrophobic surfaces (SHSs) combine a tailored nanostructure with low surface energy to trap air between surface features, excluding liquids from penetration and hindering wetting. These surfaces have drawn huge interest since the liquid repellence involves additional relevant properties, from self-cleaning to anti-icing. Concerning the frictional drag reduction effect, which is hugely promising in maritime applications, further investigations are needed to identify the key parameters controlling the interaction between SHSs and turbulent flow. With this aim, the mechanism responsible for drag variation has been analyzed by means of a properly designed experiment in a high speed recirculating channel, where a double floating plate arrangement allows for drag evaluation on both a SHS and a reference smooth one. At same time, plastron monitoring is accomplished through a high speed camera. Aluminum plates bearing different water-repellent coatings are considered. The first SHSs typology is obtained by deposition of a nanostructured hybrid coating, made of 200 nm-long boehmite lamellae creating a flower-like nanostructure, and chemically grafted fluoroalkylsilane chains (Lotus leaf approach). The second one is realized according to the SLIPS approach, infusing a fluorinated lubricant oil within the pores of the hybrid coating. Insights into the plastron properties, their evolution with time and flow velocity and their efficacy at reducing frictional drag are here presented.

Authors : D. Martínez Martínez, J. Th. M. de Hosson
Affiliations : Department of Applied Physics of the University of Groningen, Nijenborgh 4, 9747AG, Groningen, The Netherlands

Resume : The deposition of DLC films is an effective way to protect elastomers under sliding contact. The presence of the DLC film minimizes the wear and avoids the strong interaction with the counterpart caused by the tackiness of the rubber. However, the frictional behavior of the ensemble is far from being obvious, and depends strongly on the testing/operation conditions. This is because the DLC-elastomer combination is a system where the overall frictional behavior depends not only on the surface interactions, but also on the mechanical properties of the substrate. For a critical review reference is made to [1]. In this contribution, we will show how the viscoelastic properties of the rubber have an extraordinary influence on the frictional behavior of the whole ensemble. We will review several experimental results that illustrate those effects, such as load or counterpart variations. The observed phenomena are explained using a combination of adhesive (i.e. interfacial contact) and hysteresis (i.e. substrate properties) contributions. The evolution of size and shape of the contact area is used to account for the frictional behavior beyond the first lap. The role of the velocity and frequency are explored as well through ‘ad-hoc’ modeling. Finally, as a consequence of the different phenomena explained, some remarks regarding the selection of the proper elastomer depending on the operation conditions are made. [1] D.Martinez-Martinez and J.Th.M. De Hosson, Surf. Coat. Technol. 258 (2014) 677–690.

Authors : P. Zeman, M. Zitek, S. Zuzjakova, R. Cerstvy, S. Haviar, M. Kotrlova
Affiliations : Department of Physics and NTIS – European Centre of Excellence, University of West Bohemia, Univerzitni 8, 306 14 Plzen, Czech Republic

Resume : Recently, we have showed that Zr–Cu thin-film alloys can be prepared as metallic glasses in a very wide composition range (30–65 at.% Cu) by non-reactive magnetron co-sputtering. In the present study, we focus on characterization of their properties and thermal behavior in more detail. In addition, we investigate the effect of an incorporation of Hf into the Zr–Cu thin-film metallic glasses on a potential improvement of their behavior. The films were deposited using three unbalanced magnetrons equipped with Zr, Hf and Cu targets in pure Ar. The magnetron with the Zr and Hf targets were operated in a dc regime while the Cu magnetron in a high-power impulse regime. The Zr, Hf and Cu contents in the films were controlled by adjusting the dc powers and the average target power in a period, respectively. The films were deposited without an external heating onto rotating substrates. Mechanical properties of the Zr–Cu thin-film metallic glasses are strongly dependent on the elemental composition. A gradual growth of hardness with increasing Cu content up to 70 at.% correlates well with an evolution of the glass transition temperature and the crystallization temperature. The Zr–Cu films prepared with the Cu content higher than 50 at.% or at a moderate substrate bias exhibit a tendency to be more resistant to the formation of shear bands during indentation. An incorporation of Hf improves the mechanical properties of the films and the thermal stability of their glassy state.

Authors : Hyeon-Ho Jeong (1,2), Mariana Alarcón-Correa (1,3), Andrew G. Mark (1), Tung-Chun Lee (1,4), Peer Fischer(1,3)
Affiliations : (1) Max Planck Institute for Intelligent Systems, Heisenbergstrasse 3, 70569 Stuttgart, Germany; (2) Institute of Materials, École Polytechnique Fédérale de Lausanne, 1015 Lausanne, Switzerland; (3) Institute for Physical Chemistry, University of Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, Germany; (4) Institute for Materials Discovery and Department of Chemistry, University College London, Christopher Ingold Building, 20 Gordon Street, London WC1H 0AJ, United Kingdom

Resume : The electronic, optical, magnetic, and catalytic properties of nanoparticles depend on their geometry and material composition [1]. Applications in liquids and in particular water are, however, limited for a number of promising nanomaterials, as they are prone to corrosion [2,3]. Here, we present a method that can be used to protect complex hybrid 3D nanocolloids against corrosion. The method uses a nanoscale shadow growth technique, which we term ‘nano-glancing angle deposition (nanoGLAD)’ [4]. It can be used to grow three dimensional (3D) nanocolloids with some flexibility in the size, shape, and material composition of the nanoparticles. However, this scheme alone does not offer a means to prevent corrosion. Here, we show how the method can be adapted to grow 3D core-shell nanocolloids that are stable in various physiological environments [5]. We report a refined nanoGLAD scheme which, in conjunction with atomic layer deposition (ALD), can be used to protect multifunctional nanocolloids even in corrosive environments. The challenge is to ensure the complete encapsulation of the nanomaterial (core) by a defect-free shell layer. We discuss a promising metallic oxide shell layer that is chemically inert and that does not affect the colloidal stability. We demonstrate magnetic nanocolloids that without the protective layer corrode within hours in an acidic environment, but that are stable for weeks and in some cases even months when grown by the advanced nanoGLAD process. Entirely new applications are possible [6,7], including ones with Mg nanoparticles in aqueous solutions [8] and for biomedical applications at low pH [9]. [1] Y. Xia, Y. Xiong, B. Lim and S. E. Skrabalak, Angew Chem Int Ed, 2009, 48, 60-103. [2] A.-H. Lu, E. L. Salabas and F. Schüth, Angew Chem Int Ed, 2007, 46, 1222-1244. [3] A. M. Goodman, Y. Cao, C. Urban, O. Neumann, C. Ayala-Orozco, M. W. Knight, A. Joshi, P. Nordlander and N. J. Halas, ACS Nano, 2014, 8, 3222-3231. [4] A. G. Mark, J. G. Gibbs, T.-C. Lee and P. Fischer, Nat Mater, 2013, 12, 802-807. [5] H.-H. Jeong, M. Alarcón-Correa, A.G. Mark, K. Son, T.-C. Lee, and P. Fischer, Corrosion protection of nanoparticles (In preparation). [6] H.-H. Jeong, A. G. Mark, M. Alarcon-Correa, I. Kim, P. Oswald, T.-C. Lee and P. Fischer, Nat Commun, 2016, 7, 11331. [7] H.-H. Jeong, A. G. Mark, T.-C. Lee, M. Alarcón-Correa, S. Eslami, T. Qiu, J. G. Gibbs and P. Fischer, Nano Lett, 2016, 16, 4887-4894. [8] H.-H. Jeong, A. G. Mark and P. Fischer, Chem Commun, 2016, 52, 12179-12182. [9] D. Walker, B. T. Käsdorf, H.-H. Jeong, O. Lieleg and P. Fischer, Sci Adv, 2015, 1, e1500501.

Authors : Manuel Evaristo, Albano Cavaleiro
Affiliations : SEG-CEMMPRE Centre for Mechanical Engineering Materials and Processes, Department of Mechanical Engineering, University of Coimbra, Coimbra Portugal., SEG-CEMMPRE Centre for Mechanical Engineering Materials and Processes, Department of Mechanical Engineering, University of Coimbra, Coimbra Portugal.

Resume : Recent technological developments have led to the emergence of microelectromechanical systems (MEMS) and nanoelectromechanical systems (NEMS) with oscillating, rotating, and sliding contacts. Thus, it’s fundamental to improve the tribological performance to reduce stiction, friction and wear. The use of ultrathin coatings can improve the performance of those systems. In this work WS2 thin films were deposited by DC and RF magnetron sputtering with decreasing thickness from 1000 to less than 8 nm. The coatings were characterized concerning its thickness, structure and tribological performance. The roughness Ra obtained by AFM, increases with the increase of the thickness with a nonlinear growth trend. The coatings with thicknesses higher than 250 nm present a surface morphology with valleys oriented in one direction related with the shadowing effect due to the rotation of the substrates. The films were analysed by TEM in plan view, the results allows to conclude that films grow in an initial stage uniformly with the basal planes (002) parallel to the surface. Then, the growth changes to a columnar morphology with the columns having the basal planes oriented perpendicular to the films surface. The films were tribologically tested, the results showing that thickness influences the friction performance, mainly in the running in period, changes explained by the difference in the morphology through film thickness.

Authors : Petr Vasina, Pavel Soucek, Saeed Mirzaei, Vilma Bursikova, Lukas Zabransky, Mostafa Alishahi, Jiri Bursik, Vratislav Perina
Affiliations : Department of Physical Electronics, Faculty of Science, Masaryk University, Brno, Czech Republic (Petr Vasina, Pavel Soucek, Saeed Mirzaei, Vilma Bursikova, Lukas Zabransky, Mostafa Alishahi) Institute of Physics of Materials, Academy of Sciences of the Czech Republic, Brno, Czech Republic (Jiri Bursik) Nuclear Physics Institute, Academy of Sciences of the Czech Republic, v.v.i., Rez, Czech Republic (Vratislav Perina) Email:

Resume : Protective ceramic coating such as TiN, TiAlN, c-BN, etc. generally exhibit high hardness and stiffness which make them suitable for different applications. However, these coatings often suffer from brittleness and preparation of next-generation protective coatings with high hardness and moderate ductility is a current challenge in coating industry. In this regard, the ab-initio simulation have predicted that boron and carbon based coatings with a structure very similar to MAX phases can exhibit unusual combination of high stiffness and moderate ductility. In this study, the X-B-C (X=Mo and W) coatings with various compositions were deposited by co-sputtering of X, C and B4C targets at different substrate temperatures. Mid-frequency pulsed DC plasma excitation was employed to enhance the ion flux on the substrate and subsequently promote the crystallization of the coatings. The results indicate that the deposition conditions resulted in growth of partially crystalline Mo-B-C coatings with nanocomposite structure where small Mo2BC crystallites of ~ 10 nm size were embedded in an amorphous matrix. These coatings showed high hardness of 32± 1 GPa and extremely high fracture toughness. The high level of crack resistance in hard coatings observed for partially crystalline Mo-B-C coatings with nanocomposite structure is impossible to be met with commercially available coatings tested in a similar manner.

Authors : M. Dinu, L.R. Constantin, A.C. Parau, A. Vladescu, M. Braic
Affiliations : National Institute for Optoelectronics, 409 Atomistilor St., 077125, Magurele-Bucharest, Romania

Resume : Of the large class of the biocompatible coatings, those consisting of carbonitride of transition metals have been shown to fulfil to a large extent the requirements demanded for insertion into biological environment. They provide solutions to the material biocompatibility problems experienced by implantable bearing metallic surfaces, being successful in increasing the service life of the orthopaedic implants. ZrTiCN and ZrNbCN coatings, selected because each metal easily forms hard carbides and nitrides, were investigated as possible candidates for biomedical applications. The coatings were deposited on Ti based alloys, by cathodic arc evaporation technique in reactive gas mixture of Ar+CH4, and characterized for elemental (EDS) and phase (XPS) compositions, crystalline structure (HR-XRD), surface topography (SEM, AFM), hardness (nonoindentation tests) and adhesion (scratch tests). Because high corrosion resistance in body fluids is crucial for an optimal performance of biomedical devices, in vitro corrosion resistance investigation of novel biomaterials represents a compulsory requirement. The corrosion behaviour and tribo-corrosion resistance of the coatings immersed in synthetic body fluids (SBFs) were assessed and discussed in corroboration with coatings' physico-chemical and mechanical characteristics. We acknowledge the support of the Romanian Research and Innovation Ministry, project PN-III-P2-2.1-PED-2016-1580.

Authors : S. Drijkoningen1,2, P. Pobedinskas1,2, S. Korneychuk3, A. Momot1,2, A. Hardy1,2, M. Van Bael1,2, S. Turner3, J. Verbeeck3, M. Nesládek1,2, K. Haenen1,2
Affiliations : 1 Institute for Materials Research (IMO), Hasselt University, Diepenbeek, Belgium; 2 IMOMEC, IMEC vzw, Diepenbeek, Belgium; 3 Electron Microscopy for Materials Science (EMAT), University of Antwerp, Antwerp, Belgium

Resume : The preparation of diamond thin films at low temperatures (T < 410 °C) enables a wide range of novel applications, e.g. deposition on flat panel displays, plastics, and other materials that don’t withstand high temperatures. The crucial requirement for diamond growth at low temperatures is a high plasma density at low gas pressure, leading to a low thermal load onto sensitive substrate materials. Such conditions are not within reach for resonance cavity plasma systems, which typically operate at pressures above 20 mbar. Linear antenna microwave delivery systems, however, allow depositions at pressures below 1 mbar [1]. Moreover, large area deposition is feasible over substrate diameters of 30 cm. Nevertheless, the use of linear antenna microwave plasma enhanced chemical vapour deposition systems, and in particular the growth of high quality diamond layers, remains understudied. In addition, for the development of nanocrystalline structures or devices, a bottom-up approach that allows control over the obtained morphology would be highly valuable. In this work the co-deposition of high quality plates and octahedral diamond grains in nanocrystalline films is reported. In contrast to previous reports claiming the need of high temperatures (T > 1000 °C) [2], low temperatures (320 °C ≤ T ≤ 410 °C) were sufficient to deposit diamond plate structures. Cross-sectional high resolution transmission electron microscopy studies show that these plates are terminated by large {111} surface facets. Moreover, the grain boundaries are shown to be quite sharp and clean, which means there is very little disorder in between the grains. The high diamond quality is confirmed by Raman and electron energy loss spectroscopy both showing very small sp2 contributions to their respective spectra. Up to now, literature reports have focused on the characterisation of these plates and multiple growth models have been proposed [3, 4]. These models start from an initial diamond structure that contains plenty of stacking faults, i.e. layers of so-called hexagonal diamond, and account for the development of plates by preferential growth sites or by the relative growth rates of crystal facets. Nevertheless, in none of the previous reports an explicit reason for the presence of these stacking faults is given. Optical emission spectroscopy can reveal the plasma characteristics responsible for the growth mechanisms behind this particular morphology. In this work a model is proposed that accounts for the initial development of these plates full of stacking faults and the growth of this morphology at low temperatures. References 1. N. Neykova, H. Kozak, M. Ledinsky, and A. Kromka, Vacuum, 86, 6, 603–607, 2012. 2. C.-A. Lu and L. Chang, Mater. Chem. Phys., 92, 1, 48–53, 2005. 3. J. C. Angus, M. Sunkara, S. R. Sahaida, and J. T. Glass., Journal of Materials Research, 7, 11, 3001–3009, 1992. 4. H.-G. Chen and L. Chang., Journal of Materials Research, 20, 03, 703–711, 2005.

Thin films for smart applications: from organic synthesis and surface functionalization to : K. Thorwarth + Olivier Sublemontier
Authors : J.F. Pierson
Affiliations : Institut Jean Lamour (UMR CNRS 7198), Université de Lorraine, Nancy, France

Resume : The copper-oxygen binary system contains three oxides (Cu2O, Cu4O3 and CuO) that are suitable for energy applications: electrodes in Li-ion batteries, absorbent layer in solar cells, p-type transparent conductive oxide… The reactive sputtering is a powerful method to synthesize these three materials as pure phases or as mixtures. Recently, the local epitaxial growth (LEG) has been evidenced in Cu2O thin films [1]. The conditions to extend the LEG to other phases such as Cu4O3 or NiO will be discussed. Finally, the consequence of the local epitaxial growth on the microstructure of biphased copper oxide thin films will be explained. Within a given oxygen flow rate range, it is possible to grow self-assembled vertically aligned columnar Cu2O+Cu4O3 nanocomposite thin films on glass and silicon substrates at room temperature. Microstructure analyses show that each phase in nanocomposite films has the columnar growth along the whole thickness, while each column exhibits the single phase characteristics. The LEG of Cu2O is responsible for such an unusual microstructure. The intermediate oxygen flow rate between those required to synthesize single phase Cu2O and Cu4O3 films produces some Cu2O nuclei, and then the local epitaxial growth provides a strong driving force to promote Cu2O nuclei to grow sequentially, giving rise to Cu2O columns along the whole thickness. Low resistivity has been observed in such kind of nanocomposite thin films [1] Y. Wang et al., Acta Mater. 76 (2014) 207

Authors : Olivier Dalstein, Cédric Boissère, David Grosso, Andrea Cattoni, Marco Faustini
Affiliations : Olivier Dalstein, Cédric Boissère, Marco Faustini : Université Pierre et Marie Curie (UPMC) - Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP) Andrea Cattoni : CNRS - Centre de Nanosciences et de Nanotechnologies (C2N) David Grosso : Aix-Marseille Université - Institut Matériaux Microtechnologie Nanosciences de Provence (IM2NP)

Resume : We describe a new versatile route to integrate functional micro-mesoporous materials (sol-gel materials, Metal-Organic Frameworks -MOF-) into 2D photonic devices (Diffraction Gratings). The goal is to combine the original properties of micro-mesoporous materials (high porosity, sorption selectivity) and of the periodic structures (light confinement, diffraction) to achieve optical transduction for smartphone-assisted sensing of toxic vapors. A new technique called Degassing Assisted Patterning is used for the direct nano-imprinting of sol-gel thin films (SiO2, TiO2) or MOF nanoparticles, on both rigid and flexible transparent substrates. Our sensing approach relies on the monitoring of the diffracted luminosity that is directly correlated to the amount of toxic compound (alcohols, aromatic hydrocarbons…) in the atmosphere. Probing is performed by a simple smartphone or CCD camera without need of complex optical instrumentation. Unlike conventional photonic devices (mainly colorimetric), this specific configuration allows spectroscopic-like measurements. We show that sol-gel based porous homo- and hetero-structures can be fabricated and used as responsive diffraction gratings. In order to improve the selectivity towards the targeted gas, MOF nanoparticles were coupled to the sol-gel photonic device and selective detection of toxic styrene vapors was demonstrated for the first time with ZIF-8 materials at concentration as small as 58 ppm (below the permissible exposure limit).

Authors : Thibault Dufay, Raynald Seveno, Jean-Christophe Thomas, Benoit Guiffard
Affiliations : IETR UMR CNRS 6164, UBL University, University of Nantes, 2 rue de la Houssinière, 44322 Nantes Cedex 3, France ; IETR UMR CNRS 6164, UBL University, University of Nantes, 2 rue de la Houssinière, 44322 Nantes Cedex 3, France ; GeM UMR CNRS 6183, UBL University, University of Nantes, 2 rue de la Houssinière, 44322 Nantes Cedex 3, France ; IETR UMR CNRS 6164, UBL University, University of Nantes, 2 rue de la Houssinière, 44322 Nantes Cedex 3, France

Resume : Recently, the researchers’ efforts in vibration energy harvesting have focused on the development of reliable techniques of fabrication of thin-layer piezoelectric structures on flexible support. Thin films of lead zirconate titanate (PZT) have been prepared using chemical deposition on a flexible metallic substrate: a commercial aluminium (Al) foil with thickness less than 30 µm [1]. This way of fabrication is cheap and the lightness of the micro-generator makes it sensitive to air flow. To obtain high electrical energy density, the interdigitated electrodes (IDE) structure is a more efficient design than the parallel plate electrodes (PPE) and also present the advantage to operate in piezoelectric 33 mode with larger piezoelectric coefficients than in 31 mode. To realize this structure, PZT films must be separated from the aluminium ground plane before the realization of IDE. However, PZT thin films are not rigid enough to stand alone so a new substrate has to be used with a good flexibility and insulating properties. Specific polymer materials like some thermoplastics are good candidates for the new insulating and flexible substrate because of their natural flexibility. The major drawback with these soft polymers is their low resistance against thermal treatment which does not allow the direct synthesis of PZT onto polymeric substrate. The proposed solution is the transfer of the PZT thin film, obtained by classic methods, onto the polymeric substrate. This solution was used by Park et al. [2] to realize PZT on polymer, but the employed method - laser lift-off - is expensive and could be hard to transfer to the industry. In this context, a new procedure for the realization of piezoelectric PZT thin film on a polymer substrate has been developed. Starting from the PZT/Al thin film created in the laboratory, a chemical process is used to transfer the piezoelectric material to a polymer substrate. This process is cheap and would be easily transferred to the industry. In addition, with this chemical method, the metallic substrate is removed from the complete surface (~ 6 cm2) of PZT thin film in one step while the laser lift-off method requires several steps to separate PZT from the first substrate. Thus, this paper will describe the method of realization of the flexible PZT thin film on a polymer substrate. The structural (SEM, XRD, EDX) and ferroelectric characterizations of the PZT/polymer thin film carried out to check the good quality of the transferred PZT thin film will also be presented. References [1] R. Seveno and D. Averty, J. Sol-Gel Sci. Technol. 68, 175 (2013). [2] K.-I. Park, et al. Adv. Mater. 26, 2514 (2014).

Authors : Giulio Boveri, Federico Veronesi, Mariarosa Raimondo, Magda Blosi, Guia Guarini
Affiliations : Institute of Science and Technology for Ceramics

Resume : Copper or copper alloys have peculiar properties which make them suitable for a wide range of applications. In this work static and dynamic superhydrophobicity on Cu surface was achieved through a nano-engineering approach with deposition of organic/inorganic coatings made up of alumina nanoparticles - obtained by sol-gel routes - grafted by a fluoropolymer moiety. The selected processing conditions, able to control the reactivity of Cu itself, led to the formation of an homogeneous coating with a peculiar flower-like morphology, responsible for the advanced water repellence. The role of inorganic layer clearly came out since the chemical modification induced by the fluorine-rich molecule alone was not able to provide such advanced properties. Extensive SEM and XPS analyses allowed to locate the key features of the coated surfaces in the light of the most suitable annealing cycles. Heat treatments at 200 and 300°C ensured the formation of the proper morphology, while, when the temperature raises up to 400°C, CuO microwires, deleterious to superhydrophobicity, were detected. Durability tests kept unchanged the Cu performances even when low annealing temperature is concerned.

Authors : M. Boutinguiza1, M. Meixus1, R. Comesaña2, F. Lusquiños1, A. Riveiro1, J. del Val1, J. Pou1
Affiliations : 1 Applied Physics Department, University of Vigo EEI, Lagoas-Marcosende, 9. Vigo, 36310, SPAIN 2 Materials Engineering, Applied Mechanics and Construction Dpt., University of Vigo, EEI, Lagoas-Marcosende, Vigo, 36310, SPAIN.

Resume : Nanoparticles of noble metals are having great attention due to their unique response to visible and infrared radiation where their surface plasmon resonance (SPR) becomes active to enhance the optical absorption. In this work the results of obtaining TiO2/Ag films by combining the techniques of laser ablation of solids in liquids (LASL) and electrophoretic deposition in the same process are presented. Titanium oxide nanoparticles are synthetized by ablating Ti plate submerged in water while an electric field is used to deposit the nanoparticles on a conducting polymer used as electrode. The same process is repeated to ablate a silver target and deposit Ag nanoparticle on the same substrate to obtain a uniform film of TiO2/Ag. The composition, topography, crystalline structure of titanium oxide and silver nanoparticles have been studied by energy dispersive X-ray spectroscopy (EDS), high resolution transmission electron microscopy (HRTEM), X ray diffraction (XRD). UV-visible spectrometry is used to estimate the band gap of the titania colloidal solution as well as to check the optical properties of the final film. The obtained films consisted of porous coatings composed of titania and silver nanoparticles ranging from several to 60 nm and showing shift toward higher wavelengths when compared with titania films.

Coatings for biological applications 1 : Mikhael Bechelany + Mertin Stefan
Authors : K. Thorwarth
Affiliations : Empa Swiss Federal Laboratories for Materials Science and Technology CH-8600 Dübendorf, Switzerland

Resume : Diamond-like carbon (DLC) coatings are most often used successfully in a broad range of machinery applications due to their ability to improve the mechanical and chemical resistance of surfaces exposed to wear. Quite a few attempts were made to achieve similar effects in load-bearing implants such as hip, knee and spinal disc prostheses. However, several clinical studies using DLC coatings on articulating joints showed severe problems due to partial coating delamination after several years in vivo [1], which had dramatic effects for the affected patients. Such observations obviously affected the use of DLC in the MedTech field. This talk presents an overview of the main known failure mechanisms of DLC-coated medical alloys and their impact on the lifetime of the coated implant. Based on these mechanisms and using long-term tests an accurate description of the damaging processes was developed, which provides an instrument to predict the in vivo survival time and especially the long-term adhesion stability of the coating. The formation of a few atomic layers of a reactively formed interface compound, usually metal carbides, proved to be essential for reliable adhesion. Furthermore, contaminations from residual gas or any cross contamination, as they occur in standard DLC deposition processes, will result in different reactively formed interface materials with different properties. This was shown for several adhesion-promoting interlayer materials, whose sensitivity towards oxygen contamination and the corresponding impact on adhesion performance was investigated. The most promising interlayer candidate was tested in a spinal disc simulator in simulated body fluid; this interface-film optimized coating remained stable over an articulating period that corresponds to 100 years of articulation [2]. Rockwell-indentation based corrosion tests indicate a corrosion resistance of the interfaces of up to 60 years in vivo. REFERENCES: [1] R. Hauert, K. Thorwarth, G. Thorwarth, "An overview on diamond-like carbon coatings in medical applications", Surface and Coatings Technology 233, pp 119-130, year 2013. [2] K. Thorwarth, G. Thorwarth, G. R. Figi, B. Weisse, M. Stiefel, R. Hauert, “On interlayer stability and highcycle simulator performance of diamond-like carbon layers for articulating joint replacements”, International Journal of Molecular Sciences, 15(6), pp 10527-10540, year 2014.

Authors : Federico Zen, Vasilios D. Karanikolas, James Behan, Joana Vasconcelos, Jenny Andersson, Thomas Duff, Eoin M. Scanlan, Louise Bradley, Paula E. Colavita.
Affiliations : Federico Zen; James Behan; Joana Vasconcelos; Thomas Duff; Eoin M. Scanlan; Paula E. Colavita: School of Chemistry and AMBER Research Centre, University of Dublin Trinity College, College Green, Dublin, Dublin D2, Ireland. Vasilios D. Karanikolas; Louise Bradley: School of Physics and Centre for Research on Adaptive Nanostructures and Nanodevices (CRANN), University of Dublin Trinity College, College Green, Dublin, Dublin D2, Ireland. Jenny Andersson: Insplorion AB, Sahlgrenska Science Park, Medicinaregatan 8A, 413 90 Göteborg, Sweden.

Resume : Carbon materials have prompted great interest in the biomedical field due to their good performance as coating for prosthetics and medical devices. However to realize their potential it is critical to control formation and composition of the protein corona in biological media. Localized Surface Plasma Resonance (LSPR) has emerged as a powerful technique for studying the thermodynamics and the kinetics of these biological interfacial events. In this report we discuss in situ protein adsorption studies carried out at different types of carbon thin films using a recently developed LSPR sensing method. The thickness of protein layers at carbon surfaces has been calculated from experimental plasmon shifts using finite difference time domain (FDTD) simulations. These results suggest that LSPR in combination with FDTD analysis are well suited to investigating and comparing protein adsorption at carbons, even in the case of carbon materials with highly dissimilar dielectric properties. Finally, the effect of glycoside modification at carbon films in reduction protein fouling were studied using a combination of in situ and ex situ techniques.

Authors : L.Major - 1, J.M.Lackner - 2, M.Kot - 3, M. Dyner - 4, B.Major - 1
Affiliations : 1- Institute of Metallurgy and Materials Science, Polish Academy of Sciences, 30-059 Cracow, 25 Reymonta Street, Cracow, Poland; 2- JOANNEUM RESEARCH –Materials, Institute for Surface Technologies and Photonics, Niklasdorf, Austria; 3- Laboratory of Surface Engineering and Tribology, Faculty of Mechanical Engineering and Robotics, AGH University of Science and Technology, Cracow, Poland; 4- CHIRMED-Manufacturer of Surgical and Medical Instruments; 8a Mstowska Street, 42-240 Rudniki, Poland

Resume : There have been enormous strides in the development of novel metallic biomedical materials over the past three decades. There is a wide range of application of metals used in the human body. They are used as a hip knee replacements, as arterial stents and surgical plates, screws, wires and surgical instruments. Whatever be their end use, all common metals tend to react with their environments to different extents and different rates. Wear and corrosion are ubiquitous problems that affect virtually every type of surface, especially those that come in contact with other surfaces. Tribological and corrosion resistant coatings are applied in various fields of science and industry. For medical application they should withstand corrosive body fluids environment, as well as guaranty the adequate wear resistant properties. The main goal of the work was the bio- corrosion and bio- tribological properties increase together with aesthetic impression improvement of metallic surfaces by application of advanced zirconium based Zr/ZrN DLC multilayer as well as Zr-Mg-Ag(Pt) nano- composites coatings. Coatings were deposited by the use of the magnetron sputtering technique. In the frame of the work multidisciplinary coatings characterization was performed. The characterization indicated the optimum bio- tribological coating for medical tools and metallic implants application. Acknowledgment: This work was supported by the National Science Centre No: 2015/19/B/ST8/00942 and National Center of Research and Development No: DZP/M-ERA.NET-2015/285/2016

Authors : mikhael BECHELANY
Affiliations : Institut Européen des Membranes, UMR 5635 ENSCM CNRS Université Montpellier, Place Eugene Bataillon, F-34095 Montpellier cedex 5, France E-mail:

Resume : Atomic layer deposition (ALD) is a thin film technology that in the past two decades rapidly developed from a niche technology to an established method. It proved to be a key technology for the synthesis of ultrathin film, the surface modification and the fabrication of complex nanostructured materials as well as the membrane tuning. [1] In this work, we will give an overview about our activities on ALD, from the design of nanomaterials to membrane applications. After a short introduction to ALD, the versatility of the technique for the fabrication of novel nanolaminates thin films [2] and functional nanomaterials [3, 4] will be showed. Selected examples, focused on its use for the engineering of nanostructured functional materials and membranes targeting applications in water purification, biofuel cells, osmotic energy, gas separation, and health [5-8] will be discussed. [1] Advanced Materials, 2012, 24, 1017 [2] J. Phys. Chem. C, 2016, 120, 5124–5132 [3] Nano Energy 1 (2012) 696 [4] Nanoscale 7 (2015) 5794 [5] Journal of Materials Chemistry A, 2016, 4, 6487-6494 [6] Journal of Materials Chemistry A, 2016,4, 17686-17693 [7] Biosensors and Bioelectronics, 2016, BIOS-D-16-01673R1 [8] Journal of Materials Chemistry A, 2014, 2 (48), 20650 – 20658

Authors : E. Frutos, M. Karlik, T. Polcar
Affiliations : 1 Department of Control Engineering, Faculty of Electrical Engineering, Czech Technical University in Prague, Technická 2, Prague 6, Czech Republic. 2 Department of Materials, Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Trojanova 13, 120 00 Prague 2, Czech Republic. 3 National Centre for Advanced Tribology (nCATS), University of Southampton, University Road, Southampton SO17 1BJ UK.

Resume : The ideal surface modification, in form of coating, on biomaterial for orthopedic implant applications is one that exhibits excellent biocompatibility with no adverse cytotoxicity, excellent corrosion resistance, and a good combination of mechanical properties such as high strength and good fatigue resistance, low elastic modulus and good wear resistance. Sputtering techniques are extremely versatile to produce nanostructured, homogeneous, dense, compacts and crack-free coatings. This technique offers multiple possibilities in the in-situ design of complex (near) pure beta-Ti textured coatings, with body centered cubic phase (bcc), free of toxic elements. Beta-rich Ti-Nb-Zr coatings allow the combination of three different phases (alfa, alfa” and beta), depending on the concentrations of Nb and Zr, which offer the best mechanical properties a priori. The focus of this work is to design ternary coatings and their nano-mechanical characterization. Results regarding grain size, texture and residual stress magnitude of Ti-22Nb-XZr (X=10, 20, 25 w.%) as a function of conditions, will be shown. Of particular interest is the evolution of hardness, Young’s modulus and residual stress values along the thickness, manifested by Ti-22Nb-XZr, as a function of bias voltage on the substrate. It is worth highlighting how initially the young’s modulus descends from 62.86 GPa, at 0 volts, to 46.97 GPa, at -63 volts, and then progressively increases to 89.15 GPa, at -148 volts. Magnitude of residual stress will be correlated with the concentration of beta and alfa” phases, showing how the increasing bias voltage facilitates the transformation from beta to alfa”, changing compressive residual stresses magnitude from -700 MPa, at -63 volts, to -100 MPa, at -148 volts. Furthermore, it will be show as the evolution of these mechanical properties are fundamentals in the design of coatings with high fracture toughness and high wear behavior.

Authors : Rémi Mérindol [1], Rebecca Blell [1], Xiaofeng Lin [1], Matthias Pauly [1,2], Thierry Roland [1,2], Tim Lindström [3], Mikael Ankerfors [3], Christian Gauthier [1,2], Gero Decher [1,2], Olivier Félix [1]
Affiliations : [1] Institut Charles Sadron UPR22-CNRS, 23 rue du Loess, 67034 Strasbourg Cedex 2, France; [2] Université de Strasbourg, 1 rue Blaise Pascal, 67008 Strasbourg, France; [3] Innventia AB, Drottning Kristinas väg 61, Box 5604, SE-114 86 Stockholm, Sweden

Resume : Through evolution, nature has developed composite materials (e.g. bone, wood or nacre) with complex and hierarchical organization from the nano- to the macro-scale via molecular assembly. Such materials possess fascinating combinations of properties such as lightweight, strength or shock resistance by assembling hard and soft elements. Their remarkable mechanical performance at the macroscopic scale is the consequence of their hierarchical structure and the specific design at each level of organization. Among all methods available for the preparation of multifunctional nanostructured composite materials, the Layer-by-Layer technique is currently one of the most widely used due to its simplicity and versatility in combining a plethora of available nano-objects and macromolecules into finely tuned multifunctional architectures with nanometer scale control. Recently, we prepared transparent wood-inspired LbL nano-composite materials with mechanical properties challenging even medium quality steel (tensile strength around 500 MPa). The talk will illustrate some of our recent results on the design of nanostructured thin films prepared by combining hard nano-reinforcing anisotropic elements like nanofibrillated cellulose with soft polymer building blocks. Formation and growth of the different LbL-composites will be presented and their mechanical/optical properties will be discussed as a function of structure, composition, nano-object alignment and preparation conditions.

Authors : G. Benetti1,2, S. Peli1, E. Cavaliere1, M. Gandolfi1,3, C. Giannetti1, G. Ferrini1, C. Cancellieri4, M. Chiodi4, M. Van Bael2, F. Banfi1, Luca Gavioli1,*
Affiliations : 1 Interdisciplinary Laboratories for Advanced Materials Physics (I-LAMP) and Dipartimento di Matematica e Fisica, Università Cattolica del Sacro Cuore, Via dei Musei 41, 25121 Brescia, Italy 2 Katholiek Universitet, Laboratory of Solid state Physics and Magnetism, Department of Physics and Astronomy Celestijnenlaan 200D, B‐3001, Leuven, Belgium. 3 Laboratory of Soft Matter and Biophysics, Department of Physics and Astronomy, KU Leuven, Celestijnenlaan 200D, B-3001, Leuven, Belgium 4 Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Joining and Interface Technology, Überlandstrasse 129, 8600 Dübendorf, Switzerland

Resume : To make nanophase coatings based on metallic nanoparticles (NP) playing a key role in health and energy applications, one has to be able to: 1) tailor the NP properties (size, purity, crystallinity); 2) obtaining the coating directly on surfaces (type of surface, NP density); 3) understanding the coating properties (adhesion, mechanical behavior). Wet synthesis routes face the needs of colloidal stabilizers, the presence of impurities, the solvents and synthesis process costs. A flexible alternative synthesis route is the supersonic cluster beam deposition (SCBD), based on NP beams in gas phase environment. Here we show that Ag NP coatings can be deposited directly on glass or sapphire substrates via SCBD at room temperature and with a wide range of thicknesses, describing the NPs physical properties, the coating mechanical [1] and microbicidal behavior [2]. The coatings are composed of crystalline NP – with a bimodal size distribution at 6 nm and 1 nm diameter – and inter-NPs voids, the filling factor being 0.8, independently on the substrate type. The film’s density and sound velocity are 80% that of polycrystalline bulk Ag, whereas the elastic stiffness constants amount to only 50% with respect to the Ag bulk. The Ag NP coatings exert an effective and broad-spectrum bactericidal activity, both for reference strains and for a collection of clinical drug-resistant strains. [1] S. Peli et al. J. Phys. Chem. C 120 (2016) 4673 [2] E. Cavaliere et al. Nanomedicine 11 (2015) 1417

Authors : J. M. Vila-Fungueiriño1, R. Moalla2, R. Bachelet2, G. Saint-Girons2, J. Rodriguez-Carvajal3, A. Gomez4, J. Gazquez4, N. Mestres4, F. Rivadulla5, M. Gich4, A. Carretero-Genevrier1*.
Affiliations : 1Institut d´Électronique et des Systèmes (IES) UMR 5214, Bâtiment 5, 860 rue Saint Priest, 34090 Montpellier, France 2 Institut des Nanotechnologies de Lyon (INL) CNRS- Ecole Centrale de Lyon, 36 avenue Guy de Collongue, 69134 Ecully, France 3Institut Laue-Langevin, 6 rue Jules Horowitz, BP 156, 38042 Grenoble Cedex 9, France 4Institut de Ciència de Materials de Barcelona ICMAB, Consejo Superior de Investigaciones Científicas CSIC, Campus UAB 08193 Bellaterra, Catalonia, Spain 5 Centro de Investigación en Química Biológica y Materiales Moleculares (CIQUS), Universidad de Santiago de Compostela, 15782-Santiago de Compostela, Spain

Resume : The technological impact of combining substrates technologies as growing platforms with the properties of functional advanced oxides is colossal given its relevant role in the development of novel and more efficient devices. However the precise control of interfaces and crystallization mechanisms at the nanoscale of dissimilar materials need to be further developed. As an example, the integration of high quality epitaxial oxide films and nanostructures on silicon as hybrid structures rest extremely challenging because these materials are structurally and thermally different. In this light, this work describes promising strategies used to accommodate advanced oxide nanostructures and thin films on silicon substrate via chemical solution deposition approach. Divers examples will be presented separated in two different approaches i.e: (i) oxide materials entirely performed by soft chemistry, such as nanostructured piezoelectric quartz thin films on silicon [1] or ferroelectric oxide nanowires thin films epitaxially grown on silicon [2], and (ii) complex oxide materials performed by combining soft chemistry and physical techniques, such as epitaxial active perovskite oxide nanostructured thin films on silicon using the combination of soft chemistry and MBE [3,4]. As a conclusion, this presentation will cover cutting-edge strategies based on the potential of combining epitaxial growth and chemical solution deposition to develop functional oxide nanomaterials on silicon with novel structures and improved physical properties. [1] Soft chemistry based routes to epitaxial A-quartz thin films with tunables textures A.Carretero-Genevrier, M.Gich, L.Picas, J.Gazquez, , D.Grosso, C.Boissiere, J.Rodriguez-Carvajal, and Clement Sanchez. Science. Vol 340. Pp 827-831 (2013) [2] Direct Monolithic Integration of Vertical Single Crystalline Octahedral Molecular Sieve Nanowires on Silicon. A. Carretero-Genevrier, J. Oro-Sole, J. Gazquez, C. Magen, L. Miranda, T. Puig, X. Obradors, E. Ferain, C. Sanchez, J. Rodriguez-Carvajal, N. Mestres. Chemistry of Materials 26 1019 (2014) [3] Integration of functional complex oxide nanomaterials on silicon J. Vila-Fungueirio, R. Bachelet, G. Saint-Girons, M. Gendry, M. Gich, J. Gazquez, E. Ferain, F. Rivadulla, J. Rodriguez-Carvajal, N. Mestres, A. Carretero-Genevrier Frontiers in Physics 3, 38 (2015) [4] Development of Epitaxial Oxide Ceramics Nanomaterials Based on Chemical Strategies on Semiconductor Platforms A Carretero‐Genevrier et al. - Advanced Ceramic Materials, (2016)

Authors : Olivier Sublemontier Youri Rousseau
Affiliations : NIMBE, CEA, CNRS, Université Paris-Saclay, CEA Saclay 91191 Gif-sur-Yvette France

Resume : We propose a method for the elaboration, in a single step and in a confined chamber, of composite coatings made of nanoparticles embedded in a matrix. The process combines a beam of nanoparticles with Physical Vapor Deposition. The association of the two techniques is made possible by routing nanoparticles by aerodynamic means to the substrate, either immediately after their synthesis in the gas phase, or from atomized colloidal suspensions. The simultaneous deposition of the particles and the matrix is performed on the same substrate. The process allows a virtually unlimited selection in the respective chemical compositions of nanoparticles and the matrix, and a moderate temperature of the substrate. Different source types of nanoparticles are possible. A laser-driven pyrolysis reactor can be used for the in-situ synthesis. Laser pyrolysis is an efficient method to synthesize various high purity nanopowders, oxides and non-oxides, in a gas phase bottom-up approach. An atomizer that produces an aerosol from colloidal suspensions of previously synthesized nanoparticles can alternatively be used. The particle stream is formed by means of an aerodynamic lens system. This system is currently used to produce a collimated beam of particles under vacuum for further gas phase characterization or for precision 3D micro printing. It allows for long-term stable and high transmission of particles in a wide range of size and density. We show that it is possible to get an angle-controlled divergent beam of nanoaerosols by optimizing the geometry of a classical lens. In this way, homogenous deposition of nanoparticles is performed on large areas. We demonstrate the adaptation if the technique with pressure environment required for running a classical magnetron sputtering device. The later is used for depositing the material constituting the matrix of the composite film. The deposition of a large variety of materials is conceivable by this means. The possibility to elaborate large and homogenous nanostructured films were investigated with different types of nanoaerosols with different sizes and densities. Numerous application domains are already considered for this kind of nanostructured coatings, including photovoltaic, photocatalysis, aesthetic coatings, hard covering, biomedical and self-healing films. The development of the process is carried out in the frame of the HYMALAYAN project funded by the French Research National Agency (ANR) under Grant No ANR-14-CE07-0036. It is open to new potential applications.

Authors : Paulo Pedrosa, Armando Ferreira, Nicolas Martin, Mohammad Arab Pour Yazdi, Alain Billard, Filipe Vaz
Affiliations : Paulo Pedrosa: Institut FEMTO-ST, UMR 6174 CNRS, Université Bourgogne Franche-Comté, 15B Avenue des Montboucons, 25030 Besançon Cedex, France; Armando Ferreira: Centro de Física da Universidade do Minho, Campus de Gualtar, Braga, Portugal; Nicolas Martin: Institut FEMTO-ST, UMR 6174 CNRS, Université Bourgogne Franche-Comté, 15B Avenue des Montboucons, 25030 Besançon Cedex, France; Mohammad Arab Pour Yazdi: Institut FEMTO-ST, UMR 6174 CNRS, UTBM, Université Bourgogne Franche-Comté, F-90010 Belfort Cedex, France; Alain Billard: Institut FEMTO-ST, UMR 6174 CNRS, UTBM, Université Bourgogne Franche-Comté, F-90010 Belfort Cedex, France; Filipe Vaz: Centro de Física da Universidade do Minho, Campus de Gualtar, Braga, Portugal;

Resume : In the present study, inclined, zigzag and spiral TiAg and TiCu thin films were GLAD co-sputtered using two different targets, both with an opposite and oblique particle incidence angle α of 80°. The first part of this work consisted on the optimization of the sputtering pressure (varied from 0.2 to 1.5 Pa) and resulting column angle (0° ≤ β ≤ 40°), using a simple pure Ti thin film system. Afterwards, using the selected sputtering pressure (0.25 Pa), both TiAg and TiCu systems were co-sputtered with inversely changed Ti and (Ag or Cu) target currents, in order to control the obtained Ti/Ag and Ti/Cu elemental concentrations. The elaborated coatings were characterized in terms of their composition, morphology, microstructure and electrical properties. Main results show that bi-component columns can be obtained in the inclined and zigzag architectures. However, significant morphological differences are visible depending on the orientation of the sample in relation to both targets. On the other hand, rather uniform structures are achieved in the spiral nanostructures. These differences translate into interesting electrical resistivity behaviours, with higher TCR’s (1.1×10-3 and 3×10-4 °C-1 for TiCu and TiAg, respectively) obtained in the spiral structures and increased orthogonal anisotropy (Aeff = 3 and 1.4 for TiCu and TiAg, respectively) in the inclined and zigzag architectures. Keywords: TiAg, TiCu, GLAD co-sputtering, composition, electrical resistivity, anisotropy.

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Coatings for biological applications 2 : Adrian Carretero + Alberto Palmero
Authors : R. Alvarez, A. García-Valenzuela, V. Rico, A. R. Gonzalez-Elipe, A. Palmero
Affiliations : Instituto de Ciencia de Materiales de Sevilla (CSIC-US)

Resume : The oblique angle configuration has recently emerged as an invaluable tool for the deposition of porous thin films by vacuum and plasma-assisted PVD techniques. In this presentation, an up to date description of its fundamentals and nanostructuration possibilities are given, along with numerous potential applications when these films are incorporated into functional devices. Overall, the large specific surface of the layers, associated to the existence of large open micro- and mesopores, make them ideal candidates whenever an interaction with a gaseous or liquid medium is required. Applications in sensor devices, e.g. of cholesterol or glucose, or in biomedicine, where the film surface energy can be tailored to allow the growth of living cells while inhibiting bacterial proliferation, will be envisioned. Moreover, applications in optofluidics, where the optical response of multilayered structures (photonic crystals) may be tuned when different liquids pass through the porous channels, will be displayed. Results will be presented based on, but not limited to, the activities of the Nanotecnology on Surfaces research group, involving computer simulations, fundamental experiments aimed at tailoring the film porosity as well as the development of laboratory-size functional devices targeting specific applications.

Authors : S. Petralia (1), E.L. Sciuto (2), T. Cosentino (3), F. Sinatra(3), P. Fiorenza(4), C. Bongiorno(4), S. Conoci(1) and S. Libertino(4)
Affiliations : (1) STMicroelectronics, Stradale Primosole 50, 95121 Catania, Italy; (2) Dipartimento di Fisica e Astronomia, University of Catania, Catania 95100, Italy; (3) Dipartimento di Scienze Biomediche e Biotecnologiche, Via S. Sofia 87, 95100 Catania, Italy; (4) CNR-IMM Sede, Strada VIII Z.I. 5, 95121 Catania, Italy

Resume : The growing need of an early detection of diseases is driving the scientific community to find innovative and cheap DNA sensors for diagnostics. To this purpose, device miniaturization and integration in control circuitries are needed for mass production, cost reduction, and to allow the device use to non-trained people. Silicon is the most suitable substrate to be used thanks to its cheap manufacturing and high-level integration. SiO2 surfaces are used for biomolecule immobilization on Si-based sensors. Unfortunately, SiO2 suffers contamination issues in saline solution; hence, if an “active” surface is needed, e.g. for electrical transduction, SiO2 is not the best choice. Our choice was to use silicon nitride, since it is a shield to the salts ions for the electrical device under it. We developed an optimized grafting protocol on pyrolytic Si3N4 surfaces and performed an exhaustive study after each immobilization step. The surface was characterized using contact angle, ellipsometry, Atomic Force Microscopy, and Transmission Electron Microscopy. A comparison with thermally grown SiO2 surfaces chemically treated with the same immobilization protocol was also performed. DNA detections, both electrical and optical, were carried out by measuring the sensing performances of opportunely fabricated devices, DNA-microarrays and MIS-like diodes, for optical and electrical detection, respectively.

Authors : G.I. Nkou Bouala 1, A. Etiemble 2, C. Der Loughian 1, C. Langlois 1, S. Cardinal 1, J.M. Pelletier 1, J.F. Pierson 2, P. Steyer 1
Affiliations : 1 - Univ. Lyon,INSA-Lyon, MATEIS UMR CNRS 5510, 21 Avenue Jean Capelle, 69621, Villeurbanne cedex, France 2 - Institut Jean Lamour (UMR CNRS 7198), Université de Lorraine, Parc de Saurupt, 54011 Nancy, France

Resume : Thin film metallic glasses (TFMG) have recently emerged as alternative film materials for many applications, such as micro-electro-mechanical systems and biomedical use [1]. Zr-based TFMG could for example combine promising antibacterial activity and high durability to be used as coating of medical instruments to prevent hospital acquired-infections. In this way, we recently characterized a silver-rich ternary Zr-Cu-Ag TFMG [2]. Its high antibacterial activity was clearly established but some development are needed to improve its corrosion resistance. In the present study, properties optimization of micrometer-thick Zr-Cu-(Ag) TFMGs, deposited by PVD magnetron sputtering for a wide Ag-content range [0-15 at.%] using a dual-target, was investigated. The thermal stability as well as structural, microstructural, mechanical, and electrochemical properties were characterized. These films are amorphous, smooth and display high hardness and an interesting passive behavior. Finally, the antibacterial activity of these TFMGs against E. coli and S. aureus were evaluated and correlated to the composition. [1] J.P. Chu et al., Thin Film metallic glasses: Unique properties and potential applications, Thin Solid Films 520 (2012) 509-5122. [2] A. Etiemble et al., Innovative Zr-Cu-Ag thin film metallic glass deposited by PVD magnetron sputtering for antibacterial applications, J. Alloys and Comp. (2016) doi: 10.1016/j.jallcom.2016.12.259.

Authors : D.M. Vranceanu1, A. Vladescu2, M. Dinu2, T. Tran1, C.M. Cotrut1
Affiliations : 1University Politehnica of Bucharest, 313 Independeței Street, Bucharest, Romania; 2National Institute for Optoelectronics, 409 Atomistilor Street, Magurele, Bucharest, Romania;

Resume : The aim of the paper is to obtain active coatings made of silver doped hydroxyapatite with improved features on Ti6Al4V by pulsed electrochemical deposition in a single step (PED). The deposition was carried-out in a three electrode set-up as follow: Ti6Al4V – working electrode, Pt foil – counter electrode and SCE - reference electrode. The electrolyte was prepared by dissolving Ca(NO3), (NH4H2PO4) and Ag(NO3) in ultra-pure water. The deposition was performed with a potentiostat/galvanostat by pulsing the potential as follows: a potential (EON) of -2 V was applied for a period of time (tON), followed by a breaktime (tOFF) with an applied potential (EOFF) of 0V. The obtained coatings were analyzed in terms of morphology, elemental and phase composition. In order to evaluate the electrochemical behavior of the obtained coatings, electrochemical measurements have been performed in simulated body fluid (SBF) at 37 °C and pH of 7.4, in order to mimic the human body environment. The silver doped HAp active coatings were successfully achieved and confirmed by SEM-EDS and XRD analysis. Also the electrochemical investigations have confirmed that the coated samples present an improved resistance to corrosion when compared to the uncoated ones. It can be concluded that PED is an effective method for preparing Ag doped HAp coatings with balanced bioactive and antibacterial properties.

Authors : Marek Godlewski1,2, Sylwia Gieraltowska1, Lukasz Wachnicki1, Rafał Pietuszka1, Bartlomiej S. Witkowski1, Michal M. Godlewski3,4, Anna Slonska3,4, Zdzislaw Gajewski4
Affiliations : 1Institute of Physics, Polish Acad. Sci., Al. Lotników 32/46, 02-668 Warsaw, Poland 2Dept. Math. & Natural Sci. College of Sci., Card. S. Wyszynski Univ., Warsaw, Poland 3Department of Physiological Sciences, Faculty of Veterinary Medicine, Warsaw Uni-versity of Life Sciences – SGGW, Nowoursynowska 159, 02-776 Warsaw, Poland 4Veterinary Research Centre, Centre of Biomedical Research, Department of Large Animals Diseases with Clinic, Faculty of Veterinary Medicine, Warsaw University of Life Sciences – SGGW, Nowoursynowska 100, 02-797 Warsaw, Poland

Resume : Wide band gap oxides grown by Atomic Layer Deposition (ALD) method (ZnO, Al2O3, TiO2, HfO2, ZrO2) show antimicrobal activity. For the experiments we used disk diffusion method, normally used to determine drug sensitivity. Paper disks coated with thin oxide layers were tested on substrates plated with bacterial suspensions (0.5 by McFarland). Bacteria selected for experiments were chosen from reference strains and strains commonly present in hospi-tals. The highest efficiency of anti-microbal action was observed for HfO2 and ZrO2, and the lowest for TiO2. The key aspect of our method is that ALD allows coating of temperature sen-sitive materials as well as medical equipment and instruments in hospitals, dentistry and in a food industry. Thus, coating with high-k oxides, showing anti-bacterial activity, can be used in range of potential applications in medicine, veterinary, health care and food industry. This work was partially supported by the National Science Center (Decision Nos. DEC-2012/06/A/ST7/00398 and SGGW DEC-2012/05/E/NZ4/02994, 20/0139/N/ST3/04189.

Authors : Urszula Czuba ac, Robert Quintana a, Maryline Moreno-Couranjou a, Marie-Claire Gillet b, Christophe Detrembleur c, Michael Alexandre d, Patrick Choquet a
Affiliations : a- Materials Research and Technology Department, Luxembourg Institute of Science and Technology (LIST), 5, avenue des Hauts-Fourneaux, L-43623 Esch/Alzette, Luxembourg; b - Mammalian Cell Culture Laboratory, University of Liege, Allée du Six Août, 1, 4000 Liège, Belgium; c - Center for Education and Research on Macromolecules (CERM), Chemistry Department, University of Liege, 13 Allée du 6 Août, 4000 Liège, Belgium; d - Symbiose Biomaterials s.a., Avenue de l’Hopital, 1. 4000 Liège, Belgium.

Resume : Bacteria formation and colonization on biomedical interfaces can cause several adverse events, from hampering the wound healing process to cause the rejection of a medical implant. In case of metallic implants, several surface modification solutions have been extensively studied as the surface immobilization of biomolecules to control the adsorption of proteins and adhesion of cells and bacteria. Aiming at more sustainable green methodologies for surface biofuntionalization, in this communication an original, fast, solvent free and dynamic deposition process will be presented. Based on atmospheric pressure plasma dielectric barrier discharge (AP DBD) process, methacrylic-based interlayers containing highly chemically reactive quinone groups were deposited on metallic surfaces and further exploited for the covalent immobilization of bioactive enzymes. The functional layers were produced at high deposition rates, with thickness ranging from several nanometers to few microns. In addition to surface chemical and morphological characterizations, the stability of the layers was assessed through immersion tests in buffer media from pH 6 to 8. As a case study, Dispersin B, an enzyme with anti-biofilm properties, was grafted in a single step. The excellent anti-biofilm activity against staphylococcus epidermidis biofilm forming and osteoblast cells viability were found comparable to the polydopamine-based layers prepared by wet chemical methods with slow deposition rates.

Authors : Sarah Zahouani, Fouzia Boulmedais, Bernard Senger, Pierre Schaaf, Loïc Jierry, Philippe Lavalle
Affiliations : Institut National de la Santé et de la Recherche Médicale, INSERM Unité 1121, 11 rue Humann, 67085 Strasbourg Cedex, France ; Institut Charles Sadron, CNRS UPR 22, 23 rue du Lœss, 67034 Strasbourg Cedex, France; Institut National de la Santé et de la Recherche Médicale, INSERM Unité 1121, 11 rue Humann, 67085 Strasbourg Cedex, France ; Institut National de la Santé et de la Recherche Médicale, INSERM Unité 1121, 11 rue Humann, 67085 Strasbourg Cedex, France -Faculté de Chirurgie Dentaire, Université de Strasbourg, 8 rue Sainte Elisabeth, 67000 Strasbourg, France ; Institut Charles Sadron, CNRS UPR 22, 23 rue du Lœss, 67034 Strasbourg Cedex, France - University of Strasbourg Institute of Advanced Study, 5 allée du Général Rouvillois, 67083 Strasbourg Cedex, France; Institut National de la Santé et de la Recherche Médicale, INSERM Unité 1121, 11 rue Humann, 67085 Strasbourg Cedex, France -Faculté de Chirurgie Dentaire, Université de Strasbourg, 8 rue Sainte Elisabeth, 67000 Strasbourg, France

Resume : Polyelectrolyte multilayers constitute a prototype of polymeric films built by a step-by-step process. They are obtained by the alternate deposition of polyanions and polycations on solid substrates: each layer of polymer adds to the oppositely charged surface thanks to electrostatic forces, more precisely charge overcompensation (1). The buildup process appears to be extremely versatile and can be used with almost any kind of polyanion/polycation pair on almost any kind of substrate (2,3). The step-by-step technique has also been extended to other types of interactions besides electrostatic interactions between the two interacting polymers: polymer multilayers whose cohesion is based on hydrogen bonding were for example reported. In order to render multilayers mechanically more robust, multilayers based on covalent bonds between the different polymers were also developed. Covalent bonds were obtained either by first building up multilayers based on non-covalent bonds (electrostatic, hydrogen bonding...) and later by adding a cross-linking step to the film or by anchoring each polymer layer directly through covalent bonds onto the previously deposited one. This later buildup strategy is known in the literature as "covalent layer-by-layer assembly". Whereas the general laws governing the buildup of polyelectrolyte multilayers have been established (linear vs exponential growth, effect of the ionic strength on the buildup process…) only very few studies trying to establish the laws governing covalent layer-by-layer assembly have been reported so far. Here we report a study investigating the covalent layer-by-layer assembly of thin nanogel films by alternate deposition of bi- and/or tetra-functional poly(ethylene glycol) (PEG) chains bearing thiol with other chains bearing maleimide terminal groups. At the macroscopic scale, mixing PEG having maleimide terminal functions with PEG having thiol terminal functions have been demonstrated to form cross-linked biocompatible hydrogels (4). The possibility of a step- by-step buildup process to form a “nanogel” with these molecules is by far not obvious. Indeed, whereas in the case of the alternation of polyanions and polycations, electrostatic interactions can take place all along the polyelectrolyte chains, covalent bond formation requires close proximity of the two interacting groups and is thus much more restricted along the polymeric chains. On the other hand, only few interactions per chain already allows for a film construction based on covalent interactions while numerous electrostatic interactions are required for the film to be cohesive. Our goal is to investigate some rules governing the buildup of such nanogel films, their possibility to be built on different types of substrates and also to assess their capacity to be functionalized with biomolecules such as the ligand/receptor couple biotine/streptavidine. Different buildup processes resulting in the variation of several parameters as for example the length of the chains or the type of anchoring layer, have been studied using a dissipation enhanced Quartz Crystal Microbalance (QCM-D) system. (1) Decher,G.;Hong.J.D; Schmitt,J., Buildup of ultrathin multilayer films by a self-assembly process : III.. Consecutively alternating adsorption of anionic and cationic polyelectolytes on charged surfaces ,Thin Solid films, 1992, 210-211, 831-835 (2) Rios,C; Longo.J; Zahouani.S et al, A new biomimetic route to engineer enzymatically active mechano-responsive materials, Chemical Communications, 2015,51,5622-5625 (3) Zahouani, S.; Chaumont, A.; Senger, al, Stretch-induced helical conformations in Poly(L-lysine)/Hyaluronic Acid multilayers, ACS Applied Materials and Interfaces,2016,8,14958-14965 (4) Yu.J; Xu.X; Yao.F et al, In situ covalently cross-linked PEG hydrogel for ocular drug delivery applications, International Journal of Pharmaceutics, 2014,470,151-157

Authors : Aída Serrano1, Juan Rubio-Zuazo1, Jesús López-Sánchez2, Eduardo Salas-Colera1, Iciar Arnay1, Germán R. Castro1
Affiliations : 1 Spanish CRG-Spline, The European Synchrotron (ESRF), 38000 Grenoble, France and Instituto de Ciencia de Materiales de Madrid, ICMM-CSIC, 28049 Madrid, Spain; 2 Departamento de Física de Materiales, Universidad Complutense de Madrid, 28040 Madrid, Spain and Unidad Asociada IQFR (CSIC)-UCM, 28040 Madrid, Spain

Resume : Hematite (α-Fe2O3) is an antiferromagnetic material at room temperature, which presents a wide interest in diverse applications due to its low toxicity, abundance and easy control of morphology. Specifically, this iron oxide phase is a promising semiconductor for gas sensor and photocatalytic applications because its band gap is about 2.1 eV (in the range of the visible spectrum). However, the efficiency of bulk α-Fe2O3 is limited due to its low hole mobility and short carrier lifetimes. Nowadays, increasing efforts are done to tailor the physical and chemical properties of α-Fe2O3 thin films. Between the different approaches to control the final properties and improve the reactive response, the variation of thickness of the α-Fe2O3 films and using different growing substrates in terms of atomic and crystalline structure as well as the growth process is a promising option. However, it is necessary to create more insight in the mechanism that define the physical and chemical properties. The influence of the charge carriers at the interface between the thin film and the substrate is crucial but the crystallinity, morphology and the film orientation as well. In this work, we evaluate the growth factors of α-Fe2O3 single crystalline thin films deposited by Pulsed Laser Deposition (PLD) on three different substrates: STO (111), α-Al2O3 (0001) and LaAlO3 (001). An exhaustive study of morphological and structural properties of thin films and the possible formation of other phases at the film/substrate interface has been carried out. For that, several techniques has been employed: Grazing Incidence Surface X-Ray Diffraction (GIXRD), X-ray Photoelectron Spectroscopy (XPS), X-ray Absorption Spectroscopy (XAS), Atomic Force Microscopy (AFM) and Raman Spectroscopy. Moreover, we present preliminary results about the efficiency of these α-Fe2O3 thin films as gas sensor for CO and CH4 gas from the conductance measurements, which are correlated with their morphological and structural properties.

Authors : Joana M. Vasconcelos, Federico Zen, James Behan, Khairul Hoque, Ronan J. Cullen, Paula E. Colavita
Affiliations : School of Chemistry and Centre for Research on Adaptive Nanostructures and Nanodevices (CRANN), Trinity College Dublin, College Green, Dublin 2, Ireland.

Resume : Carbon materials are widely used in medical applications in the form of nanodiamonds, carbon dots, carbon nanotubes and diamond like carbons. The excellent performance of carbon-based biomaterials is attributed in part to the unique and desired physico-chemical properties of these materials. However, the origin of their desirable bioresponse is not yet fully understood and there is currently great interest in understanding what role carbon surface chemistry might play in determining the great performance of carbon as a biomaterial. In this work we present a detailed study of the physico-chemical properties of disordered carbon and carbon-modified thin films. A combination of spectroscopic and microscopic techniques was used to characterise carbon thin films composition, topography, surface charge density, wettability and surface free energy. X-ray photoelectron spectroscopy (XPS), contact angle, atomic force microscopy (AFM), ellipsometry and surface zeta potential methods were utilised to characterise four types of disordered carbon surfaces: amorphous carbon (a-C), hydrogen doped amorphous carbon (a-C:H), oxidised amorphous carbon (a-C:O) and carbohydrate-modified amorphous carbon (a-C:Lac). The four disordered carbon surfaces were further incubated in biological media and a relation between carbon surface chemistry, wettability and charge density and carbon bioresponse was established.

Authors : F.G. Cougnon, A. Lamberti, D. Depla
Affiliations : Department of Solid State Sciences, Ghent University, Krijgslaan 281(S1) 9000 Gent, Belgium ; Department of Materials Science & Engineering, Ghent University, Technologiepark-Zwijnaarde 903 9052 Zwijnaarde, Belgium ; Department of Solid State Sciences, Ghent University, Krijgslaan 281(S1) 9000 Gent, Belgium

Resume : A composite material is a heterogeneous material which consists of clearly distinguishable phases, often referred to as the reinforcement and the matrix. The purpose of a composite is to combine the properties of its constituting building blocks in order to obtain a material with enhanced mechanical properties. Fibre-reinforced polymer-matrix composites have higher specific stiffness and strength compared to metals, as well as better resistance against corrosion and fatigue. Therefore, these materials are very attractive for lightweight applications such as aeronautics, space applications, transport, automotive sector, sports and recreation. High-quality composite components are often produced by autoclave-assisted curing. The quality of the final composite component is strongly influenced by the conditions of the autoclave cycle, i.e. cure time, pressure and temperature. To assure optimal quality of the composite part, there is a growing demand for sensors that are capable of in-situ monitoring of the curing process during the autoclave cycle. Thin-film thermocouples (TFTCs) are promising candidates to fulfill in-situ temperature sensing. Unlike more conventional fibre-, foil- or micro-sensors causing material and geometrical discontinuities when embedded in the composite material, TFTCs can be embedded without major impact on the composite?s structural life, integrity and mechanical properties. Furthermore TFTCs have negligible mass, a high degree of geometrical freedom and minimal gas flow disturbance when applied on a surface. In this work, the influence of the deposition parameters during magnetron sputtering of the TFTC on its performance (Seebeck coefficient) is presented together with a fundamental understanding of the performance of the TFTC in relation to thin film microstructure and properties.

Authors : C. Tudisco, A. L. Pellegrino, G. Malandrino, G. G. Condorelli
Affiliations : Dipartimento di Scienze Chimiche, Università di Catania and INSTM UdR di Catania, Italy

Resume : The multiferroic bismuth ferrite (BFO) has attracted enormous attention since it shows ferroelectric/piezoelectric behavior, magnetic transition temperature well above room temperature and a rather low direct band gap (about 3 eV) which make this material suited for a wide range of potential applications such as advanced data storage devices, spintronics, sensors and energy harvesting. MOCVD grown ferroelectric BFO films have been covalently functionalized with optically active molecular monolayers based on either Eu(beta-diketonates) complexes or systems with delocalized pi-greek electrons (namely free and metaled tetra-carboxyphenyl porphyrins ) adopting a highly versatile multi-step approach. BFO films were deposited by MOCVD using a multi-metal source, consisting of the Bi(phenyl)3, and Fe(tmhd)3 (phenyl = –C6H5, H-tmhd = 2,2,6,6-tetramethyl-3,5-heptandione) precursor mixture and were characterized using X-Ray Diffraction, Scanning Electron Microscopy, Energy Dispersive X-Ray microanalysis, while the piezoelectric response of deposited films has been investigated at the nanoscale by Piezoelectric Force Microscopy. BFO surface functionalization route consists of a prefunctionalization step with bi-functional phosphonic linkers (phosphonoproprionic and aminopropylphosphonic acids), having terminal carboxylic and amino groups able to bind the molecular layers. Molecular modified surfaces were studied by X-Ray Photoelectron and fluorescence spectroscopies.

Authors : Mavin Motay, David Martel, Olivier Felix, Valérie Keller, Gero Decher, Nicolas Keller
Affiliations : Institut de Chimie et Procédés pour l’Energie, l’Environnement et la Santé (ICPEES), CNRS, Strasbourg University, 25 rue Becquerel 67087 Strasbourg, France; Institut Charles Sadron (ICS), CNRS, Strasbourg University, 23 rue du Loess 67034 Strasbourg, France

Resume : Interest in Layer-by-Layer (LbL) self-assembly thin films has been growing for the past decade. This coating technique consists in the alternating deposition of oppositely charged species on charged surface, providing new or complementary properties to a material. Due to the easy processing of this construction, the LbL coating technique can be transferred on different types and more complex surfaces whilst preserving the properties of the films. Here, we report on the construction of photocatalytic nanoscale films containing positively charges titanium dioxide (TiO2) nanoparticles and polystyrene sulfonate polyanion on model surfaces (Si wafer, quartz slides), as well as on polyester textiles, using both dipping and spraying methods. Both dipped/sprayed films exhibit a linear growth according to the number of pair of layer built on model surfaces, with a film growth monitored by ellipsometry, Quartz Crystal Microbalance, UV-Vis Diffuse Reflectance spectroscopy and microscopy. SEM analysis showed a homogeneous and porous coating of TiO2 nanoparticles, already for one single layer pair. The LbL construction was further transferred to textiles for self-decontaminating photocatalytic applications. The influence of thin film properties on their photocatalytic activity was studied taking the formic acid oxidation under UV-A light as model test reaction for indoor air remediation. Catalyst–saving nanoscale thin films with a single layer pair showed very high photocatalytic activity.

Authors : Matteo Ghidelli (a), Luca Mascaretti (a), Tarek Afifi Afifi (a), Beatrice R. Bricchi (a), Valeria Russo (a), Carlo S. Casari (a,b), Roberto Matarrese (c), Isabella Nova (c), Andrea Li Bassi (a,b)
Affiliations : (a) Micro- and Nanostructured Materials Laboratory, Department of Energy, Politecnico di Milano, via Ponzio 34/3, 20133, Milano, Italy. (b) Center for Nanoscience and Technology – IIT@Polimi, via Giovanni Pascoli 70/3, 20133, Milano, Italy (c) Laboratory of Catalysis and Catalytic Processes, Department of Energy, Politecnico di Milano, via La Masa 34, 20156, Milano, Italy

Resume : The integration of Plasmonic (metal) Nanoparticles (P-NPs) within wide band gap semiconductors is object of investigations for the possibility to enhance the performance of photovoltaic or photocatalytic thin film devices. Nevertheless, the mechanisms of coupling between plasmons and light within such nanostructures is not fully understood and key questions involving the effect of P-NPs size and dispersion still require in-depth studies. Moreover, P-NPs are often produced by liquid phase techniques and then embedded within the semiconductor film, limiting the control of the obtained structures. Here, we use vapor phase Pulsed Laser Deposition (PLD) to produce Au P-NPs and nanostructured TiO2 photoanode films. By varying the process parameters and exploiting annealing treatments, we tune Au P-NPs size distribution and the hierarchical TiO2 nanoscale morphology. Optimized Au P-NPs are coupled with TiO2, involving deposition of P-NPs at the bottom or at the top of the TiO2 as well as co-deposition of integrated TiO2/Au-NPs assemblies or multilayers. For the different architectures, we show that the plasmonic peak of Au NPs affects the optical behavior of TiO2, improving light absorption by promoting multiple-reflections and scattering. In the case of co-deposition, we show that the TiO2 growth, morphology and optical properties are affected by the Au NPs. For the best optimized systems, we discuss the results of the photocatalytic performance under solar simulator illumination.


Symposium organizers
José Filipe VAZUniversity of Minho, Physics Department

Campus de Gualtar, 4710-057 Braga, Portugal
Martin FENKERfem Forschungsinstitut Edelmetalle + Metallchemie

Plasma-Oberflächentechnik/ Material-Physik, Katharinenstr. 17, 73525 Schwäbisch Gmünd, Germany
Philippe STEYER (Main organizer)INSA de Lyon – MATEIS Laboratory

7 av. Jean Capelle - Bât. B. Pascal - 69621 Villeurbanne Cedex - France
Tomas POLCARUniversity of Southampton

Highfield, Southampton SO17 1BJ, U.K.