ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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hardness and hence abrasion protection tends to be lower. Dependent on the deposition parameters, the properties of a-C:H:Me can be varied over wide ranges: From metal-like and carbide-like to amorphous-carbon-like. On the one hand this allows to a certain extent the adaption of the coating’s mechanical properties to the load-carrying and overload capability required by the targeted application. On the other hand, this offers the opportunity to use these coatings for the realization of tailored friction properties. In the present study, tungsten-modified hydrogenated amorphous carbon coatings (a-C:H:W) were deposited on hardened and tempered tool steel using an industrial scale coating machine. The applied coating technique was reactive magnetron sputtering of a tungsten carbide (WC) target in argon-acetylene atmosphere. To improve the adhesion to the substrate, a thin chromium layer and a WC intermediate layer were deposited by arc evaporation and magnetron sputtering, respectively. For the deposition of the a-C:H:W functional layer, four process parameters, namely cathode power, bias voltage, process gas pressure and argon-to-acetylene flow ratio were varied according to a 2 4 factorial design. The coated samples were characterized in terms of structural, mechanical and tribological properties: Micro structure and thickness were evaluated by scanning electron microscopy. Surface roughness was measured using a profilometer. Hardness and Young’s modulus were determined by instrumented indentation tests. Rockwell C indentation and scratch tests provided information on cracking resistance and adhesion to the substrate. Friction and wear of the coatings were studied in ball-on-disk tests over a sliding distance of 1,000 meters (13,263 rotations). In dry sliding against 100Cr6 balls, coefficients of friction in the range of 0.10 to 0.43 were determined for the respective coatings. Under oil lubrication, the respective friction coefficient was found to be between 0.05 and 0.11. For almost any of the tested coatings, the observed friction behavior was also sufficiently stable. This proves the potential of providing tailored friction properties by proper choice of the deposition parameters of a-C:H:W coatings. 4:50pm B4-3-10 Characterization of Plasma Electrolytic Oxidation (PEO) Coatings on 6082 Aluminium Alloy, A. Jarvis, A. Yerokhin (A.Yerokhin@sheffield.ac.uk), University of Sheffield, UK, P. Shashkov, Cambridge Nanolytic, Ltd., UK, A. Matthews, University of Sheffield, UK This research characterizes two sets of PEO alumina coatings obtained on BS 6082 series aluminium alloy substrates. One was produced using the more common electrolyte containing silicates, and the other was made without silicates. The coatings were characterized using a variety of methods and their relative wear resistance was evaluated with a reciprocating wear tester. The wear resistance of the coating made using the advanced method is significantly higher than the reference coating. The greater wear resistance of this coating appears to be due to the difference in wear modes: mostly transverse fracture cracks that lead to a gradual loss of material. The silicate containing coating suffers a more severe wear mode of both transverse as well as lateral cracks leading to spalling. The difference in wear resistance appears to be due to both higher micro-scale Vickers indentation hardness, as well as its greater indentation toughness that indicates the resistance to the formation of lateral cracks, and thus spalling. The reasons for this difference in toughness were not determined. The greater hardness of the new coating is likely due to lower porosity. Nanoindentation hardness measurements were used to evaluate the hardness and elastic modulus at a nano scale and tend to support the difference in alpha and gamma alumina phase content found using XRD measurements. Several other coating characteristics were investigated and appeared to have no correlation with wear resistance. The residual stresses in the coatings were measured using two methods: XRD and an optical fluorescence method (piezo-spectroscopic) which both showed the same trends. An attempt was made to quantify the amount of amorphous alumina in the coatings using a quantitative Rietveld method, however the results were inconclusive due to the difficulty in determining the exact gamma alumina phase crystal structure, thought to be a defect spinel structure. 5:10pm B4-3-11 The microstructure and mechanical properties of Cr- Si-Ti-Al-N coatings, Y.C. Kuo, National Taiwan University of Science and Technology, Taiwan, J.W. Lee (jefflee@mail.mcut.edu.tw), C.J. Wang, Ming Chi University of Technology, Taiwan The Cr-Si-Ti-Al-N thin films with various silicon contents were fabricated by a co-sputtering process with three targets. The influences of silicon contents on the microstructure, mechanical and tribological properties of Cr-Si-Ti-Al-N films were investigated in this work. The phase structures of the coatings were determined by a glancing angle X-ray diffractometer (GA-XRD). The microstructures of thin films were evaluated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The hardness and elastic modulus were examined by a nanoindentation. The scratch test, Rockwell-C adhesion and pin-on-disk wear tests were used to evaluate the adhesion quality and tribological properties of thin films. It was found that the column structure was transformed to a dense Wednesday Afternoon, April 25, 2012 64 structure when the silicon contents were higher than 10 at.%. The hardness and tribological properties were also strongly influenced by the silicon concentration of the Cr-Si-Ti-Al-N coatings. Hard Coatings and Vapor Deposition Technology Room: Royal Palm 1-3 - Session B5-2 Hard and Multifunctional Nano-Structured Coatings Moderator: J. Paulitsch, Christian Doppler Laboratory for Application Oriented Coating Development at the Department of Physical Metallurgy and Materials Testing, Montanuniversitӓt Leoben, Austria, R. Sanjines, Ecole Polytechnique Fédérale de Lausanne, Switzerland, P. Zeman, University of West Bohemia, Czech Republic 1:50pm B5-2-1 Tribological properties of Cr0.65Al0.35N-Ag selflubricating hard coatings from room temperature to 550 °C, C. Mulligan (c.mulligan@us.army.mil), U.S. Army ARDEC, Benet Laboratories, US, P. Papi, Rensselaer Polytechnic Institute, J. Lin, W. Sproul, Colorado School of Mines, US, D. Gall, Rensselaer Polytechnic Institute Cr0.65Al0.35N-Ag composite layers, 5-μm-thick and containing 10-15 at.% Ag, were deposited by reactive magnetron co-sputtering from Cr, Al, and Ag targets on Si(001) and 440C stainless steel substrates. The layer composition was controlled by the relative power to sputtering targets. The layers exhibit a nanocomposite structure with segregated Ag grains homogeneously distributed throughout a CrAlN matrix. The tribological properties against alumina counterface were evaluated from testing temperatures, Tt = 25-550 °C in ball-on-disk dry sliding operation. Cr0.65Al0.35N-Ag composite layers demonstrate low friction (
duration for super-low friction seems to be a big issue for its application. DLC based nanocomposite coatings are promising to solve the problems. In this work, pure DLC coatings on Ti-6Al-4V plates and Si wafers were firstly investigated using direct ion beam deposition technique in order to optimize the processing parameters. Then, nanocomposite coating samples of DLC-MoS2 were deposited on the Ti-based substrate by a hybrid technique of ion beam deposition and target biased ion beam sputtering. The structure of the nanocomposite samples were investigated by Raman Spectroscopy, X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). Their mechanical and tribological properties were studied using nanoindentation, scratch testing, nanoanalyzer, and pin-ondisc. The results show that the nanocomposite coatings have much improved adhesion to the substrate and comparable hardness and tribological properties with that of pure DLC coatings. 3:10pm B5-2-5 Growth of Amorphous Hf-Al-Si-N Thin Films by DC Magnetron Sputtering, H. Fager (hanfa@ifm.liu.se), Linköping University, IFM, Thin Film Physics Division, Sweden, A. Mei, University of Illinois at Urbana-Champaign, US, B.M. Howe, Air Force Research Laboratory, US, J.E. Greene, I. Petrov, University of Illinois at Urbana- Champaign, US, L. Hultman, Linköping University, IFM, Thin Film Physics Division, Sweden Crystalline and nanocrystalline transition metal nitrides have attracted a lot of interest over the years, and they are well known to have a wide range of outstanding properties that makes them suitable in many different applications. In comparison with crystalline transition metal nitrides, and also compared to corresponding carbides and oxides, very little has been reported on amorphous transition metal nitrides and most of their properties are still unknown. Nevertheless they are potentially attractive, e.g., as wear resistant coatings, due to their homogeneous structure. We propose amorphous multicomponent transition metal nitrides as a new class of refractory materials. Using kinetically limited growth techniques - including low growth temperatures and high deposition rates - is one of the keys to growing amorphous transition metal nitride films. In this study, we investigate the HfN-AlN-Si3N4 system, where the difference in atomic size and bond coordination between the constituent elements, in combination with kinetically limited growth, promotes the formation of an amorphous structure. Hf1-x-yAlxSiyN thin films were grown on Si(001) substrates by reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target. We show that we can control the film morphology, from nanocrystalline to amorphous, by varying the ion flux and growth temperature, and also the film composition by varying the ion energy. Compositional analysis of the as-deposited films was performed by energy dispersive x-ray spectroscopy (EDS), and the structural information was gained by x-ray diffraction and analytical transmission electron microscopy. We will report on hardness and elastic properties of the films, as well as temperature dependent resistivity. 3:30pm B5-2-6 Nanocomposite coatings in the Al-Ge-N system: synthesis, structure and mechanical and optical properties, E. Lewin (erik.lewin@empa.ch), M. Parlinska-Wojtan, J. Patscheider, Empa, Switzerland Coatings in the Al-Ge-N system have been synthesized using reactive DC magnetron sputtering and characterized with the goal to explore the structure and properties, as well as their potential use as hard optical coatings. The composition was varied from pure AlN to pure GeNy. Also experiments varying substrate temperature and sample bias were conducted. Coatings were analyzed using X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and scanning and transmission electron microscopy. Besides the binary reference samples, ternary samples with Ge-contents from 5 to 30 at.% were synthesized, and found to be nanocomposites of a nanocrystalline, Ge-containing AlN-phase, nc-(Al1-xGex)N, and an amorphous, N-deficient GeNy-phase. The grain size of the (Al1-xGex)N phase decreased with increasing Ge-content from about 30 to 15nm. Additionally the (Al1-xGex)N -phase was found to exhibit two different textures depending on the Ge-content: at low Ge content a (001) preferred orientation was observed, while at increased Ge-content the (110) orientation became dominant. The GeNy phase was found to be highly susceptible to sputter damage during sputter-cleaning prior to XPS analysis. A nanocomposite-hardening, similar to what has been observed for e.g. the AlN/Si3N4 system, was observed: the hardness increased from 19 GPa (for the AlN reference sample) to 25 GPa for the hardest ternary sample. Samples were found to have a high transparency in the visible region, and the index of refraction shows a slight dependence of Ge-content, increasing from about 2.0 to 2.2 as Ge-content increases from 0 to 30 at.%. Thus these coatings have a potential use as protective coatings for optical components operating in the visual or near IR range. 3:50pm B5-2-7 Shape- Recovery of Thin Film Metallic Glasses Upon Annealing, C. Rullyani, C. Li, J. Chu (jpchu@mail.ntust.edu.tw), National Taiwan University of Science and Technology, Taiwan Thin film metallic glasses (TFMGs) possess many excellent and unique properties, including high strength, ductility, annealing-induced amorphization and good adhesion between the substrate and film. Like ordinary metallic glasses, the TFMGs in general undergo the glass transition and crystallization at temperatures of Tg and Tx, respectively, upon annealing. Another exceptional property of TFMGs is the shape-recovery ability during annealing at temperatures between Tg and Tx (or so-called the supercooled liquid region, ΔT) due mainly to the low viscosity flow. Surface defects such as indentation marks on the scales up to a few micrometers tend to shrink in size or even disappear without crystallization in ΔT. In this study, 200 nm-thick TFMGs with different compositions are deposited on Si substrates. Nanoindentation tests are performed to evaluate the film properties. Surface morphology and microstructure before and after annealing within ΔT are examined and reveal that the size of indentation mark decreases after annealing. As a result, the shape-recovery behavior is confirmed and detailed characterization results of various TFMGs as a function of annealing time will be discussed. Keyword: thin film metallic glass, annealing, shape recovery 4:10pm B5-2-8 Thin Film Metallic Glasses: Unique Properties and Potential Applications, J. Chu (jpchu@mail.ntust.edu.tw), National Taiwan University of Science and Technology, Taiwan INVITED A new group of thin film metallic glasses (TFMGs) have been reported to exhibit properties different from conventional crystalline metal films, though their bulk forms are already well-known for the high strength and toughness, large elastic limits, excellent corrosion and wear resistances because of the amorphous structure. In recent decades, bulk metallic glasses (BMGs) have gained a great deal of interest due to the substantial improvements in specimen sizes. On the other hand, much less attention has been devoted to the TFMGs, despite the fact that they have many properties and characteristics which are not readily achievable with other types of metallic or oxide films. Furthermore, these TFMGs have been progressively used for engineering applications and thus deserve to be recognized in the field of thin film coatings. In addition, while the BMGs are still difficult to use because of their brittle macroscopic nature and difficulty of processing, TFMGs are a possible solution to make use of their great properties of high strength, large plasticity, and excellent wear resistance. In this presentation, many advantages and properties of TFMGs are discussed. These are such as mechanical properties, tribological properties, annealing-induced amorphization and resulting smooth surface, some of which lead to useful applications, for example, for substrate fatigue property enhancements. In addition, potential applications in microelectronics and optoelectronics are mentioned. Ironically, there have been enormous research efforts dedicated to developing metallic glasses with large critical sizes only to reveal that the best use for these materials may, in fact, be in thin film applications. It is thus hoped that this talk serves the purpose of calling attention to the importance of TFMGs such that many more studies and applications may be explored. 4:50pm B5-2-10 Improving the corrosion resistance and hardness of TaN films by silicon addition, G. Ramírez (enggiova@hotmail.com), S.E. Rodil, S. Muhl, G. Galicia, Universidad Nacional Autónoma de México - Instituto de Investigaciones en Materiales, Mexico, E. Camps, L. Escobar- Alarcón, Instituto Nacional de Investigaciones Nucleares de México, México, D. Solis-Casados, Universidad Autónoma del Estado de México - Centro de Investigación en Química Sustentable, Mexico The aim of the present work was to obtain dense thin films that present simultaneously good corrosion resistance and hardness. For this, we propose the deposition of nanocomposite thin films where tantalum nitride (TaN) nanocrystals were embedded in an amorphous silicon nitride (SiNx) phase. The deposition was done using two magnetrons; one of pure Si and the other of pure Ta and the amount of Si into the samples was varied by changing the RF power (20 - 340 W) applied to the Si target. The N2/Ar ratio was fixed at the value optimized for the stoichiometric deposition of tantalum nitride films (6/14). The TaN-SiNx samples were deposited on silicon and their composition, structure and hardness were evaluated by Xray photoelectron spectroscopy, X.ray diffraction and nanoindentation, respectively. The results indicated that the silicon content increased linearly from 1 to 12 at% as the RF power was increased. Meanwhile, the hardness showed a maximum around 5.4 at% of silicon attaining 40 GPa, representing a 20 % hardness enhancement in comparison to the fcc phase of the TaN film. From the structural analysis, it was observed that the TaN d -fcc phase was stabilized due to the addition of Si. However, for the 65 Wednesday Afternoon, April 25, 2012
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I C M C T F 2 0 1 2 INTERNATIONAL C
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TABLE OF CONTENTS Welcoming Remarks
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2012 ICMCTF SCHEDULE OF EVENTS DAY
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SYMPOSIUM A Coatings for Use at Hig
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Marco Cremona Pontificia Universida
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Exhibitor Keynote Lecture Tuesday,
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2011/12, discuss ideas and prioriti
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At the focus topic, from the experi
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2012 R.F. Bunshah Annual Award & IC
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ICMCTF 2012 Graduate Student Awards
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ICMCTF 2012 thanks Plansee for thei
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ICMCTF 2012 thanks AJA Internationa
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ICMCTF 2012 thanks CemeCon for thei
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ICMCTF 2012 Short Courses April 22
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ICMCTF 2012 Planning Grid We provid
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Key to Session/Paper Numbers A Coat
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Monday Morning, April 23, 2012 Fund
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New Horizons in Coatings and Thin F
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Fundamentals and Technology of Mult
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Advanced Characterization of Coatin
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Hard Coatings and Vapor Deposition
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Tribology & Mechanical Behavior of
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Coatings for Use at High Temperatur
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Applications, Manufacturing, and Eq
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Wednesday Afternoon, April 25, 2012
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Thursday Afternoon Poster Sessions
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Free Caricatures & Massages!! E-1 V
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ICMCTF 2012 EXHIBIT HALL Internatio
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I C M C T F 2012 S P O N S O R S Bo
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All in Good Measure A 24 µm scan o
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Call For Abstracts Deadline: MAY 2,
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CC800 ® /9 HIPIMS true integration
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Exhibit Hall Reception - Atlas Ball
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Kaufman & Robinson announces their
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Miba Coating Group is the specialis
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PLANSEE SE, 6600 Reutte, Austria, T
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� ��
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Plenary Talk Room: Golden Ballroom
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content. Analyses of the oxidised c
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- The control on the gradient in re
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μ = 0.4 to μ = 0.9). On the other
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application tests the ta-C coated d
Page 113 and 114: 4:10pm C2-2/F4-2-10 Investigation o
Page 115 and 116: process with surfactant on WO3/ITO
Page 117 and 118: is already reported. To further com
Page 119 and 120: conditions. The details of the comp
Page 121 and 122: esidual stress and to the Poisson
Page 123 and 124: Coatings for Use at High Temperatur
Page 125 and 126: eactive gases with the target mater
Page 127 and 128: Hard Coatings and Vapor Deposition
Page 129 and 130: emerging fields. State-of-the-art t
Page 131 and 132: transparent conducting layers. Howe
Page 133 and 134: methods provide similar carrier den
Page 135 and 136: of AISI 52100 steels by developing
Page 137 and 138: deposition based on high power puls
Page 141 and 142: coatings removed from the aluminum
Page 143 and 144: spectroscopy varies from 25 at% to
Page 145 and 146: This article describes how to use s
Page 147 and 148: een demonstrated both theoretically
Page 149 and 150: Furthermore, the silane coupling ag
Page 151 and 152: 10:40am A1-1-9 High temperature oxi
Page 153 and 154: 10:40am B4-2-10 Understanding the d
Page 155 and 156: 11:00am B5-1-10 Hard nanocrystallin
Page 157 and 158: * Sandia National Laboratories is a
Page 159 and 160: fluidized bed of tin, zinc and alum
Page 163: mechanical and chemical properties.
Page 167 and 168: stainless steel DIN X42Cr13 surface
Page 169 and 170: 2:30pm TS1-1-3 Surface engineering
Page 173 and 174: Hard Coatings and Vapor Deposition
Page 175 and 176: X-ray diffraction patterns of the Z
Page 177 and 178: 11:20am B6-1-11 Direct current magn
Page 179 and 180: loading situations could help to ob
Page 181 and 182: Energetic Materials and Micro-Struc
Page 183 and 184: The present work was supported by t
Page 185 and 186: silica-based hydrophilic coatings i
Page 187 and 188: extent depending on the actual grow
Page 189 and 190: [1] F. Tasnádi, B. Alling, C. Hög
Page 191 and 192: eproducibility of the preparation o
Page 193 and 194: showed by the uncoated 4140 steel s
Page 195 and 196: polarization resistance and corrosi
Page 197 and 198: thin films in which a multiscale mo
Page 199 and 200: centers, ascribed to conduction ele
Page 201 and 202: BP-26 Characterization of laser abl
Page 203 and 204: BP-38 Stress signature of an amorph
Page 205 and 206: simultaneously optimize materials p
Page 207 and 208: CP-17 Effects of UV Light Treatment
Page 209 and 210: amorphous structure with a smooth s
Page 211 and 212: addition, it was observed that the
Page 213 and 214: EP-5 The effective Indenter concept
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the substrates directly or after ra
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as-grown films using textured Si as
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proposed memory device exhibits exc
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FP-24 Effect of hydrogen addition o
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oxide obtained was correlated to th
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Post Deadline Discoveries and Innov
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chemical bonds have also been achie
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9:40am B3-1-6 Compressive stress ge
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10:20am D2-1-8 Corrosion Resistance
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property combination is attractive
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PVD is a challenging task. The pres
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Chang, G.W.: C2-3/F4-3-3, 29; GP-3,
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Huang, K.H.: BP-33, 102 Huang, P.H.
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Moody, N.R.: F6-1-1, 7 Moon, S.: D1
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Szeremley, D.: G3-1-7, 68 Szesz, E.
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NOTES 145
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Description of Research Highlights:
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their presentations in order to eva
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NOTES 151
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153
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