ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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properties, composition and surface morphology were investigated as a function of the Si + kinetic energy. These properties were studied using the following characterization techniques: Raman spectroscopy, X-ray diffraction, nanoindentation, X-ray Photoelectron Spectroscopy and Scanning Electron Microscopy. It was found that the Si content, which was varied from 1.6 to 3.5 at.%, depends, approximately linearly, on the silicon ion kinetic energy. Ti-Si-N films with hardness as high as 34.0 GPa, which is suitable for many mechanical applications, were obtained. The hardness was strongly affected by the silicon ion energy, and there exists an optimal energy value, and consequently a certain value of Si content at which the maximum hardness is reached. These results show that the properties of the deposited material are controlled partially by the Si + kinetic used for thin film growing. BP-20 The Role of Aluminium for the Nanostructure and Mechanical Properties of Sputtered Ti-B Films, P. Epaminonda, University of Cyprus, Cyprus, K. Polychronopoulou, Northwestern University, US, K. Fadenberger, Robert Bosch GmbH, Germany, M. Baker, University of Surrey, UK, P. Gibson, Joint Research Centre, Italy, A. Leyland, A. Matthews, University of Sheffield, UK, P.H. Mayrhofer, Montanuniversität Leoben, Austria, C. Rebholz (claus@ucy.ac.cy), University of Cyprus, Cyprus TiB2 thin films have been studied extensively due to their outstanding properties (e.g. high hardness, high thermochemical stability), making them highly attractive for many applications in erosive, abrasive, corrosive and/or high-temperature environments. Despite their excellent properties, the usability and commercialisation of TiB2 films has been mainly hindered due to their brittleness and limited film-substrate adhesion, caused by the primarily strong covalent bonding in the hexagonal B network and the high compressive stresses developed in deposited films on various substrates. An effective route for improving adhesion and toughness in hard ceramic films is the introduction of ductile metal additions (e.g. Al) or layers, therefore modifying their bonding type and structure. In this study, TixAlyB2 thin films (0.88≤ x ≤1.04; 0.12≤ y ≤0.31), with Al contents between 4.1-9.4 at.%, were deposited onto Si (100) and AISI 316 stainless steel substrates by simultaneous co-sputtering from TiAl and TiB2 targets in an argon discharge at 170˚C. The coating stoichiometry, relative phase composition, nanostructure, density and mechanical properties were determined using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Laser Acoustic Surface Waves (LAwave), in combination with nanoindentation measurements. It is shown that Al substitutes for Ti in stoichiometric closed-packed hexagonal nanocrystalline thin films with 4.1 at.% Al, having an average grain size of 2-3 nm. As the Al concentration is increased, the crystallinity, average TiB2 grain size, density, hardness and elastic modulus decreases from ~2-3 to 1 nm, 4.2 to 3.8 g/cm 3 , 32.9 to 20.6 GPa and 335 to 250 GPa, respectively, while the film adhesion increases. Density and elastic modulus from ab initio calculations are compared to experimental results. The elastic modulus values measured by nanoindentation are lower than the calculated ab initio data, attributable to the nanocrystalline nature of the deposited films. BP-21 Microstructural characteristics of CrZrSiN coatings synthesized by unbalanced magnetron sputtering with CrZrSi segment targets, Kim, S.Y. Lee (sylee@kau.ac.kr), Korea Aerospace University, Republic of Korea Segment target have several advantages and theoretically it is possible to deposit almost all materials and to synthesize various multicomponent coatings without much difficulties. It does however remains a bigh challenge to control the composition and microstructure of the coatings synthesized using segment targets. In this work, CrZr-Si-N films were synthesized by unbalanced magnetron sputtering with CrZrSi segment target. Three type segment targets with various volumne ratios of (Cr+Zr) and Si (each ratio is 11:1vol%, 5:1vol% and 3:1vol %) used in this work. Characteristics such as crystalline structure, surface morphology, hardness and chemical composition as a function of the Si content were investigated by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscope(TEM), atomic force microscopy (AFM), microhardness tester, and glow discharge optical emission spectroscopy (GDOES). The surface images of the coatings were revealed that the coatings have dense and compact microstructure and very smooth surface and the surface roughness decreased as Si content in the coatings increased. The microstructure of coatings were consisted of mainly Cr(Zr)N crystalline and Si3N4 amorphous. The hardness of films approximately 32GPa was maintained up to 10% Si content and further increase in Si contents above 10% in the coatings seemed to decrease the hardness of the coatings below approximately 24GPa. Detailed experimental result will be presented. Thursday Afternoon Poster Sessions 100 BP-22 Synthesis and characterization of CrZrAlN coatings synthesized by unbalanced magnetron sputtering, J.Y. Kim (kimjjyu@naver.com), D.J. Kim, B.S. Kim, S.Y. Lee, Korea Aerospace University, Republic of Korea The Cr-Zr-N films have much improved mechanical properties and very smooth surface roughness. However, even though their outstanding properties, the Cr-Zr-N coatings revealed their mechanical properties deteriorated severely with increasing Zr content at 500� due to very rapid oxidation. Addition of Al into the CrZrN coatings is expected to improve the high temperature properties of the coatings as Al provides excellent oxidation resistance the Cr-Zr-N coatings. In this study, the quaternary Cr- Zr-Al-N films with various Al contents were synthesized using CrZrAl segment target by unbalanced magnetron sputtering. The characteristics of films were investigated by X-ray diffraction (XRD), Field Emission- Scanning Electron Microscope (FE-SEM), atomic force microscopy (AFM), glow discharge optical emission spectroscopy (GDOES), and microhardness tester. Preliminary results show that the Cr-Zr-Al-N coatings had outstanding mechanical properties with various Al contents at high temperature especially high temperature thermal stability of the coatings. Detailed experimental results will be presented. BP-23 Mechanical Performance and Nanoscaled Deformation of Bias- Sputtered (AlCrTaTiZr)NCy Multi-component Coatings, S.Y. Lin, S.Y. Chang (shouyi@dragon.nchu.edu.tw), Y.C. Huang, F.S. Shieu, National Chung Hsing University, Taiwan This work develops (AlCrTaTiZr)NCy multi-component carbo-nitride films, with the incorporations of quinary metallic elements, nitrogen and carbon, as protective hard coatings by co-sputtering of AlCrTaTiZr alloy and graphite in an Ar/N2 mixed atmosphere with the application of different substrate biases. All the (AlCrTaTiZr)NCy films deposited at different conditions exhibited a simple face-centered cubic structure. As the applied substrate bias and graphite-target power increased, the deposited (AlCrTaTiZr)NCy coatings transformed from a large columnar structure with a (111) preferred orientation to a nanocrystalline or even nearamorphous structure. With increasing substrate bias and graphite-target power, the hardness and H/E ratio of the coatings increased from 18 GPa and 0.07, to much higher values of about 32 GPa and 0.12, respectively, attributed to the densification of the coatings, the introduction of covalentlike carbide bonds, the refinement of grains and the formation of nanocomposite structure. Because of the severe lattice distortions in the multi-component coatings caused by the addition of differently-sized atoms, the dominant deformation mechanism of the coatings was found to be the formation of stacking faults, rather than complete dislocations only. BP-24 Effects of Substrate Temperature and Bias-Voltage on Mechanical Properties and Oxidation Resistance of TiAlYN Films, N. Hattori (sunmoonstone@live.jp), Keio University, Japan, T. Takahashi, Yungaloy Corporation, Japan, M. Noborisaka, T. Mori, M. Takahashi, T. Suzuki, Keio University, Japan It is well known that TiAlN films have been preferred in cutting tools for their mechanical properties and good oxidation resistance. However, many studies have reported that they oxidize over 800 ºC. The addition of another element into matrix is one of the techniques to improve the properties. In our previous researches, we reported on the effect of yttrium addition to TiAlN films and investigated the mechanical and thermal properties. It was concluded that the films with the yttrium content 2 at.% showed the highest hardness and excellent oxidation resistance up to 900ºC. In this study, we synthesized Ti49Al49Y2N films changing substrate temperatures at 100ºC, 200ºC, 300ºC, 400ºC and bias-voltages at 50 V, 100 V, 200 V, 300 V and investigated their oxidation resistance and mechanical properties. The films were deposited on Si, WC-Co, and SUS304 substrates by the cathodic arc ion plating (AIP) method. The hardness and adhesion were analyzed by a micro-Vickers hardness tester and Rockwell hardness tester, respectively. For the evaluation of the oxidation resistance, X-ray diffraction (XRD) and glow discharge optical emission spectrometry (GDOES) were performed to identify oxide layers of the films annealing at 900ºC for 1 hour in air. The hardness of all films doped yttrium increased, they were about 33 GPa. The films deposited at a substrate temperature of 200ºC showed an excellent substrate adhesion and oxidation resistance. The difference in hardness and oxidation resistance was not observed changing bias-voltage. The results demonstrated that Ti49Al49Y2N films deposited at bias voltage at 100 V and substrate temperature at 200ºC showed high hardness and the oxidation resistance keeping the adhesion strength.
BP-26 Characterization of laser ablation bismuth and iron oxide plasmas used for deposition of bismuth-iron-oxide thin films, E. Camps (eecamps2@hotmail.com), D. Cardona, L. Escobar-Alarcon, National Institute for Nuclear Research, Mexico, S. E. Rodil, Mexican National Autonomous University, Mexico Bismuth-Iron-Oxides (BFO) can be grown in five different phases, which can have very important multiferroic, magneto-optical and optoelectronic properties, making them attractive for different technological applications. The synthesis of these materials in the form of thin films has become quite difficult, being the laser ablation technique one of the most suitable. In the present work, it is proposed the simultaneous ablation of two targets (Bi and Fe2O3) in a reactive atmosphere (containing O2), in order to deposit BFO thin films with different compositions. Prior to deposition, the plasma parameters, such as, mean kinetic ion energy (Ep), plasma density (Np) and the type of excited species, were studied, in an attempt to correlate these parameters with the properties of the deposited BFO thin films. Deposition of the thin films was carried out at room temperature and the working pressure was varied in the range between 10 and 50 mTorr with an Ar/O2 =80/20 gas mixture. The iron oxide (FO) plasma parameters were kept constant at Ep (FO) = 100 eV and Np(FO) = 2 x 10 13 cm -3 , whilst the bismuth plasma parameters were varied in the range between 30 and 300 eV for the Ep(Bi) and 8 x 10 11 – 9 x 10 13 cm -3 for the Np(Bi). The optical emission spectroscopy (OES) showed that the most abundant excited species present in the plasmas were neutral Fe and neutral, once and three times ionized Bi. The deposited samples were characterized by Raman spectroscopy, X-Ray diffraction, EDS and RBS. The properties of the films are presented as a function of the plasma parameters. BP-27 A study of W/DLC/WSC composite films fabricated by magnetron sputtering method, M. Dai (daimingjiang@Tsinghua.org.cn), C. Wei, S. Lin, H. Hou, K. Zhou, Guangdong General Research Institute of Industrial Technology, China WS2 is well known for its solid lubricating behavior in industry applications. However, it is sensitive to environmental atmosphere. In humid ambient air, WS2 gets easily oxidized, resulting in the deterioration of its tribological properties. Moreover, another problem of the sputtered WS2 films is their very low adhesion to the substrate, which lead in most cases to poor wear behaviour. In order to improve the properties of WS2 film in humid air conditions, W/DLC/WSC composite films have been fabricated by magnetron sputtering method. The properties of composite films, as well as the influence of C content in the WSC top layers were researched. The morphology and microstructure of the composite films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Vickers microhardness tests were carried out to determine the hardness of composite films. Scratch tests were performed to study the adhesion of the films to the cemented carbide substrate. The tribological behavior was investigated using a ball-on-disk tribometer in humid air. The results show that the composite films exhibit dense and featureless in appearance. None C or WS2 peaks have been observed in the spectrum of X-ray diffraction (XRD). Thereby, amorphous or nanocrystal structure has been obtained according to the SEM and XRD results. The hardness of composite films can be enhanced obviously and it increases with increasing the C content. Compared to the pure WSx film, W/DLC/WSC gradational structure can improve the adhesion of films effectively and the maximal critical load of the composite film reaches 62N. Though the friction coefficient of the pure WSx film (about 0.1) is lower than that of the composite films (0.15~0.25), the wear life of composite films are much longer owning to their higher hardness and better adhesion to the substrate. BP-28 Comparison of the wear characteristics of TIN Coating with Manganese Phosphate Coating., S. Sivakumaran (ilaiyavel@svce.ac.in), A. Alangaram, Sri Venkateswara College of Engineering, India Manganese Phosphate is an Industrial coating used to reduce friction and improve lubrication in sliding components. In this study, the tribology behavior of TIN (which as produce both PVD and CVD ) Manganese Phosphate with Molybdenum disulphide (MoS2) coated AISID2 steels was investigated. The Surface morphology of manganese phosphate coatings was examined by Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscopy (EDX) .The wear tests were performed in a pin on disk apparatus as per ASTM G-99 Standard. The wear resistances of the coated steel were evaluated through pin on disc test using a sliding velocity of 3.3 m/s under Constant load of 50 N and controlled condition of temperature and humidity. The Coefficient of friction and wear loss were evaluated. The temperature rise after 15 min and 30 min were recorded for each load. Wear pattern of TIN, Manganese Phosphate with Molybdenum disulphide (MoS2) coated pins were captured using Scanning Electron Microscope (SEM). Based on the results of the wear test the manganese phosphate with Molybdenum disulphide (MoS2) coating exhibited the lowest coefficient of friction and the lowest wear loss under 50 N load. BP-29 Exotic mechanical properties of Cu-doped nano-columnar DLC coating, S. Yukawa (mb11052@shibaura-it.ac.jp), T. Aizawa, Shibaura Institute of Technology, Japan Diamond like carbon (DLC) coating has grown up to be a common way to improve the surface properties of dies and punches in dry stamping, by its high wear resistance and low friction coefficient. Aiming at its applications to an oxide-glass stamping mold-dies or a protective coating for MEMS/NEMS, high thermal stability and elasticity are much required. In fact, the stability above the glass-transition temperature of oxide glass and nano-scaled dimensional guaranty are needed in the mold-stamping process of collective lens for solar panel. Nano-columnar DLC coating is suitable for this application because of the high durability and metallic doping is effective to improve the thermal stability at elevated temperature. Cu-doped DLC coating was prepared on silicon wafer by RF-sputtering with co-doping method. Deposited film was subjected to low energy electron beam (EB) irradiation. Nano-columnar structure with copper, which segregates into the grain boundary, is formed. The size of columns ranges around 20 nm. Raman spectroscopy is utilized to describe the bonding state and structure. Obtained spectrum of Cu-doped EB irradiated film is deconvoluted into two peaks pairs (D1:G1, D2:G2) . Calculated I(D1)/I(G1) and I(D2)/I(G2) are 2.11 and 0.30, respectively. D1 and G1 correspond to initial amorphous carbon matrix: its in-plain correlation length (La) becomes 2 nm. La ( D2:G2) is estimated 15 nm and it nearly equals to average of the measured diameter of columns. That is, graphitization takes place in the inter-columnar region and vertically aligned graphitic network is embedded in the disordered amorphous carbon matrix. Compared with undoped sample after EB irradiation, Cu-doped sample is much more graphitized: I(D2)/I(G2) for undoped is 0.46. Hardness of the samples, Cu-doped after EB, undoped as-deposited and undoped after EB, obtained by nano-indentation are 1166, 1150 and 1071, respectively. Cu-doped sample shows a great elastic recovery and it is reversible up to 12% of the film thickness. This hardening and elasticity attribute to segregation of copper and graphitization in inter-columnar region. BP-30 A Fem Supported Method for the Fast Determination of Nanoindenter’s Tip Geometrical Deviations, K.-D. Bouzakis (bouzakis@eng.auth.gr), M. Pappa, G. Maliaris, Michailidis, Aristoteles University of Thessaloniki; Fraunhofer Project Center Coatings in Manufacturing (PCCM), Greece Nanoindentation is an effective technique for determining mechanical properties of bulk materials and thin films. Prevailing measurement uncertainties in nanoindentations by Vickers or Berkovich diamond pyramids are commonly caused by manufacturing imperfections of the indenter’s side angles and tip sharpness. Moreover, the tip geometry changes during the indenter lifetime, due to diamond wear. The present paper deals with a fast method for estimating diamond indenters’ tip nano and micro geometry. On one hand, this method is based on a combination of nanoindentations on Si(100) used as reference material and on the other hand, on FEM supported calculations of Martens hardness. The hardness calculations are conducted using equivalent indenter tip geometry with geometrical characteristics which may vary for a specific set of parameters, describing the real indenter with manufacturing imperfections. These parameters are varied in successive iterations until the calculated hardness converges with that of the reference material. For a quick determination of these parameters, the software package “TIDE” (TΙp Deviations Estimation) has been developed. “TIDE” is based on numerous FEM supported simulation’s results of nanoindentations onto the reference material varying the indenter tip geometry. By this software package, a quick prediction of nanoindenters’ tip equivalent geometry is facilitated, also for anticipating changes due to wear of the diamond over time. KEYWORDS: Nanoindentation, tip, imperfections, wear BP-31 An analysis of the effect of local environments on vacancy formation and diffusion energy barriers in Ti0.5Al0.5N alloy, F. Tasnádi (tasnadi@ifm.liu.se), M. Odén, I. Abrikosov, Linköping University, Sweden Microstructure analysis has attracted high interest in hard coating developments as often the microstructure has a decisive impact on the hardness of materials [1]. For example, the isostructural spinodal decomposition results in hardness enhancement in TiAlN. Modeling microstructure evaluation via diffusion requires not only energetic, mechanical but also kinetic parameters of the materials. Here we present results on vacancy, divacancy formation and migration in Ti0.5Al0.5N alloy using first principles density functional theory calculations. We pay special attention to the analysis of the impact of local environments. [1] P. H. Mayrhofer, C. Mitterer, L. Hultman and H. Clemens, Prog. Mat. Sci. 51, 1032 (2005). 101 Thursday Afternoon Poster Sessions
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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
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4:10pm C2-2/F4-2-10 Investigation o
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process with surfactant on WO3/ITO
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is already reported. To further com
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conditions. The details of the comp
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esidual stress and to the Poisson
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eactive gases with the target mater
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emerging fields. State-of-the-art t
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transparent conducting layers. Howe
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methods provide similar carrier den
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of AISI 52100 steels by developing
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deposition based on high power puls
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coatings removed from the aluminum
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spectroscopy varies from 25 at% to
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This article describes how to use s
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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 161 and 162: Coatings for Use at High Temperatur
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Page 165 and 166: duration for super-low friction see
Page 167 and 168: stainless steel DIN X42Cr13 surface
Page 169 and 170: 2:30pm TS1-1-3 Surface engineering
Page 171 and 172: Coatings for Use at High Temperatur
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
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Page 185 and 186: silica-based hydrophilic coatings i
Page 187 and 188: extent depending on the actual grow
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Page 207 and 208: CP-17 Effects of UV Light Treatment
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Page 213 and 214: EP-5 The effective Indenter concept
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Page 225 and 226: Post Deadline Discoveries and Innov
Page 227 and 228: chemical bonds have also been achie
Page 229 and 230: 9:40am B3-1-6 Compressive stress ge
Page 231 and 232: 10:20am D2-1-8 Corrosion Resistance
Page 233 and 234: property combination is attractive
Page 235 and 236: PVD is a challenging task. The pres
Page 237 and 238: Chang, G.W.: C2-3/F4-3-3, 29; GP-3,
Page 239 and 240: Huang, K.H.: BP-33, 102 Huang, P.H.
Page 241 and 242: Moody, N.R.: F6-1-1, 7 Moon, S.: D1
Page 243 and 244: Szeremley, D.: G3-1-7, 68 Szesz, E.
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NOTES 151
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