ICMCTF 2012! - CD-Lab Application Oriented Coating Development
ICMCTF 2012! - CD-Lab Application Oriented Coating Development
ICMCTF 2012! - CD-Lab Application Oriented Coating Development
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properties, composition and surface morphology were investigated as a<br />
function of the Si + kinetic energy. These properties were studied using the<br />
following characterization techniques: Raman spectroscopy, X-ray<br />
diffraction, nanoindentation, X-ray Photoelectron Spectroscopy and<br />
Scanning Electron Microscopy. It was found that the Si content, which was<br />
varied from 1.6 to 3.5 at.%, depends, approximately linearly, on the silicon<br />
ion kinetic energy. Ti-Si-N films with hardness as high as 34.0 GPa, which<br />
is suitable for many mechanical applications, were obtained. The hardness<br />
was strongly affected by the silicon ion energy, and there exists an optimal<br />
energy value, and consequently a certain value of Si content at which the<br />
maximum hardness is reached. These results show that the properties of the<br />
deposited material are controlled partially by the Si + kinetic used for thin<br />
film growing.<br />
BP-20 The Role of Aluminium for the Nanostructure and Mechanical<br />
Properties of Sputtered Ti-B Films, P. Epaminonda, University of<br />
Cyprus, Cyprus, K. Polychronopoulou, Northwestern University, US, K.<br />
Fadenberger, Robert Bosch GmbH, Germany, M. Baker, University of<br />
Surrey, UK, P. Gibson, Joint Research Centre, Italy, A. Leyland, A.<br />
Matthews, University of Sheffield, UK, P.H. Mayrhofer, Montanuniversität<br />
Leoben, Austria, C. Rebholz (claus@ucy.ac.cy), University of Cyprus,<br />
Cyprus<br />
TiB2 thin films have been studied extensively due to their outstanding<br />
properties (e.g. high hardness, high thermochemical stability), making them<br />
highly attractive for many applications in erosive, abrasive, corrosive and/or<br />
high-temperature environments. Despite their excellent properties, the<br />
usability and commercialisation of TiB2 films has been mainly hindered due<br />
to their brittleness and limited film-substrate adhesion, caused by the<br />
primarily strong covalent bonding in the hexagonal B network and the high<br />
compressive stresses developed in deposited films on various substrates. An<br />
effective route for improving adhesion and toughness in hard ceramic films<br />
is the introduction of ductile metal additions (e.g. Al) or layers, therefore<br />
modifying their bonding type and structure.<br />
In this study, TixAlyB2 thin films (0.88≤ x ≤1.04; 0.12≤ y ≤0.31), with Al<br />
contents between 4.1-9.4 at.%, were deposited onto Si (100) and AISI 316<br />
stainless steel substrates by simultaneous co-sputtering from TiAl and TiB2<br />
targets in an argon discharge at 170˚C. The coating stoichiometry, relative<br />
phase composition, nanostructure, density and mechanical properties were<br />
determined using X-ray photoelectron spectroscopy (XPS), X-ray<br />
diffraction (XRD) and Laser Acoustic Surface Waves (LAwave), in<br />
combination with nanoindentation measurements. It is shown that Al<br />
substitutes for Ti in stoichiometric closed-packed hexagonal nanocrystalline<br />
thin films with 4.1 at.% Al, having an average grain size of 2-3 nm. As the<br />
Al concentration is increased, the crystallinity, average TiB2 grain size,<br />
density, hardness and elastic modulus decreases from ~2-3 to 1 nm, 4.2 to<br />
3.8 g/cm 3 , 32.9 to 20.6 GPa and 335 to 250 GPa, respectively, while the<br />
film adhesion increases. Density and elastic modulus from ab initio<br />
calculations are compared to experimental results. The elastic modulus<br />
values measured by nanoindentation are lower than the calculated ab initio<br />
data, attributable to the nanocrystalline nature of the deposited films.<br />
BP-21 Microstructural characteristics of CrZrSiN coatings synthesized<br />
by unbalanced magnetron sputtering with CrZrSi segment targets,<br />
Kim, S.Y. Lee (sylee@kau.ac.kr), Korea Aerospace University, Republic of<br />
Korea<br />
Segment target have several advantages and theoretically it is possible to<br />
deposit almost all materials and to synthesize various multicomponent<br />
coatings without much difficulties. It does however remains a bigh<br />
challenge to control the composition and microstructure of the coatings<br />
synthesized using segment targets. In this work, CrZr-Si-N films were<br />
synthesized by unbalanced magnetron sputtering with CrZrSi segment<br />
target. Three type segment targets with various volumne ratios of (Cr+Zr)<br />
and Si (each ratio is 11:1vol%, 5:1vol% and 3:1vol %) used in this work.<br />
Characteristics such as crystalline structure, surface morphology, hardness<br />
and chemical composition as a function of the Si content were investigated<br />
by X-ray diffraction (XRD), field emission scanning electron microscope<br />
(FE-SEM), transmission electron microscope(TEM), atomic force<br />
microscopy (AFM), microhardness tester, and glow discharge optical<br />
emission spectroscopy (GDOES). The surface images of the coatings were<br />
revealed that the coatings have dense and compact microstructure and very<br />
smooth surface and the surface roughness decreased as Si content in the<br />
coatings increased. The microstructure of coatings were consisted of mainly<br />
Cr(Zr)N crystalline and Si3N4 amorphous. The hardness of films<br />
approximately 32GPa was maintained up to 10% Si content and further<br />
increase in Si contents above 10% in the coatings seemed to decrease the<br />
hardness of the coatings below approximately 24GPa. Detailed<br />
experimental result will be presented.<br />
Thursday Afternoon Poster Sessions 100<br />
BP-22 Synthesis and characterization of CrZrAlN coatings synthesized<br />
by unbalanced magnetron sputtering, J.Y. Kim (kimjjyu@naver.com),<br />
D.J. Kim, B.S. Kim, S.Y. Lee, Korea Aerospace University, Republic of<br />
Korea<br />
The Cr-Zr-N films have much improved mechanical properties and very<br />
smooth surface roughness. However, even though their outstanding<br />
properties, the Cr-Zr-N coatings revealed their mechanical properties<br />
deteriorated severely with increasing Zr content at 500� due to very rapid<br />
oxidation. Addition of Al into the CrZrN coatings is expected to improve<br />
the high temperature properties of the coatings as Al provides excellent<br />
oxidation resistance the Cr-Zr-N coatings. In this study, the quaternary Cr-<br />
Zr-Al-N films with various Al contents were synthesized using CrZrAl<br />
segment target by unbalanced magnetron sputtering. The characteristics of<br />
films were investigated by X-ray diffraction (XRD), Field Emission-<br />
Scanning Electron Microscope (FE-SEM), atomic force microscopy (AFM),<br />
glow discharge optical emission spectroscopy (GDOES), and microhardness<br />
tester. Preliminary results show that the Cr-Zr-Al-N coatings had<br />
outstanding mechanical properties with various Al contents at high<br />
temperature especially high temperature thermal stability of the coatings.<br />
Detailed experimental results will be presented.<br />
BP-23 Mechanical Performance and Nanoscaled Deformation of Bias-<br />
Sputtered (AlCrTaTiZr)NCy Multi-component <strong>Coating</strong>s, S.Y. Lin, S.Y.<br />
Chang (shouyi@dragon.nchu.edu.tw), Y.C. Huang, F.S. Shieu, National<br />
Chung Hsing University, Taiwan<br />
This work develops (AlCrTaTiZr)NCy multi-component carbo-nitride films,<br />
with the incorporations of quinary metallic elements, nitrogen and carbon,<br />
as protective hard coatings by co-sputtering of AlCrTaTiZr alloy and<br />
graphite in an Ar/N2 mixed atmosphere with the application of different<br />
substrate biases. All the (AlCrTaTiZr)NCy films deposited at different<br />
conditions exhibited a simple face-centered cubic structure. As the applied<br />
substrate bias and graphite-target power increased, the deposited<br />
(AlCrTaTiZr)NCy coatings transformed from a large columnar structure<br />
with a (111) preferred orientation to a nanocrystalline or even nearamorphous<br />
structure. With increasing substrate bias and graphite-target<br />
power, the hardness and H/E ratio of the coatings increased from 18 GPa<br />
and 0.07, to much higher values of about 32 GPa and 0.12, respectively,<br />
attributed to the densification of the coatings, the introduction of covalentlike<br />
carbide bonds, the refinement of grains and the formation of<br />
nanocomposite structure. Because of the severe lattice distortions in the<br />
multi-component coatings caused by the addition of differently-sized atoms,<br />
the dominant deformation mechanism of the coatings was found to be the<br />
formation of stacking faults, rather than complete dislocations only.<br />
BP-24 Effects of Substrate Temperature and Bias-Voltage on<br />
Mechanical Properties and Oxidation Resistance of TiAlYN Films, N.<br />
Hattori (sunmoonstone@live.jp), Keio University, Japan, T. Takahashi,<br />
Yungaloy Corporation, Japan, M. Noborisaka, T. Mori, M. Takahashi, T.<br />
Suzuki, Keio University, Japan<br />
It is well known that TiAlN films have been preferred in cutting tools for<br />
their mechanical properties and good oxidation resistance. However, many<br />
studies have reported that they oxidize over 800 ºC. The addition of another<br />
element into matrix is one of the techniques to improve the properties. In<br />
our previous researches, we reported on the effect of yttrium addition to<br />
TiAlN films and investigated the mechanical and thermal properties. It was<br />
concluded that the films with the yttrium content 2 at.% showed the highest<br />
hardness and excellent oxidation resistance up to 900ºC.<br />
In this study, we synthesized Ti49Al49Y2N films changing substrate<br />
temperatures at 100ºC, 200ºC, 300ºC, 400ºC and bias-voltages at 50 V, 100<br />
V, 200 V, 300 V and investigated their oxidation resistance and mechanical<br />
properties. The films were deposited on Si, WC-Co, and SUS304 substrates<br />
by the cathodic arc ion plating (AIP) method. The hardness and adhesion<br />
were analyzed by a micro-Vickers hardness tester and Rockwell hardness<br />
tester, respectively. For the evaluation of the oxidation resistance, X-ray<br />
diffraction (XRD) and glow discharge optical emission spectrometry<br />
(GDOES) were performed to identify oxide layers of the films annealing at<br />
900ºC for 1 hour in air.<br />
The hardness of all films doped yttrium increased, they were about 33 GPa.<br />
The films deposited at a substrate temperature of 200ºC showed an<br />
excellent substrate adhesion and oxidation resistance. The difference in<br />
hardness and oxidation resistance was not observed changing bias-voltage.<br />
The results demonstrated that Ti49Al49Y2N films deposited at bias voltage at<br />
100 V and substrate temperature at 200ºC showed high hardness and the<br />
oxidation resistance keeping the adhesion strength.