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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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duration for super-low friction seems to be a big issue for its application.<br />

DLC based nanocomposite coatings are promising to solve the problems. In<br />

this work, pure DLC coatings on Ti-6Al-4V plates and Si wafers were<br />

firstly investigated using direct ion beam deposition technique in order to<br />

optimize the processing parameters. Then, nanocomposite coating samples<br />

of DLC-MoS2 were deposited on the Ti-based substrate by a hybrid<br />

technique of ion beam deposition and target biased ion beam sputtering.<br />

The structure of the nanocomposite samples were investigated by Raman<br />

Spectroscopy, X-ray photoelectron spectroscopy (XPS) and X-ray<br />

diffraction (XRD). Their mechanical and tribological properties were<br />

studied using nanoindentation, scratch testing, nanoanalyzer, and pin-ondisc.<br />

The results show that the nanocomposite coatings have much<br />

improved adhesion to the substrate and comparable hardness and<br />

tribological properties with that of pure DLC coatings.<br />

3:10pm B5-2-5 Growth of Amorphous Hf-Al-Si-N Thin Films by DC<br />

Magnetron Sputtering, H. Fager (hanfa@ifm.liu.se), Linköping<br />

University, IFM, Thin Film Physics Division, Sweden, A. Mei, University<br />

of Illinois at Urbana-Champaign, US, B.M. Howe, Air Force Research<br />

<strong>Lab</strong>oratory, US, J.E. Greene, I. Petrov, University of Illinois at Urbana-<br />

Champaign, US, L. Hultman, Linköping University, IFM, Thin Film<br />

Physics Division, Sweden<br />

Crystalline and nanocrystalline transition metal nitrides have attracted a lot<br />

of interest over the years, and they are well known to have a wide range of<br />

outstanding properties that makes them suitable in many different<br />

applications. In comparison with crystalline transition metal nitrides, and<br />

also compared to corresponding carbides and oxides, very little has been<br />

reported on amorphous transition metal nitrides and most of their properties<br />

are still unknown. Nevertheless they are potentially attractive, e.g., as wear<br />

resistant coatings, due to their homogeneous structure. We propose<br />

amorphous multicomponent transition metal nitrides as a new class of<br />

refractory materials.<br />

Using kinetically limited growth techniques - including low growth<br />

temperatures and high deposition rates - is one of the keys to growing<br />

amorphous transition metal nitride films. In this study, we investigate the<br />

HfN-AlN-Si3N4 system, where the difference in atomic size and bond<br />

coordination between the constituent elements, in combination with<br />

kinetically limited growth, promotes the formation of an amorphous<br />

structure. Hf1-x-yAlxSiyN thin films were grown on Si(001) substrates by<br />

reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target. We show<br />

that we can control the film morphology, from nanocrystalline to<br />

amorphous, by varying the ion flux and growth temperature, and also the<br />

film composition by varying the ion energy.<br />

Compositional analysis of the as-deposited films was performed by energy<br />

dispersive x-ray spectroscopy (EDS), and the structural information was<br />

gained by x-ray diffraction and analytical transmission electron microscopy.<br />

We will report on hardness and elastic properties of the films, as well as<br />

temperature dependent resistivity.<br />

3:30pm B5-2-6 Nanocomposite coatings in the Al-Ge-N system:<br />

synthesis, structure and mechanical and optical properties, E. Lewin<br />

(erik.lewin@empa.ch), M. Parlinska-Wojtan, J. Patscheider, Empa,<br />

Switzerland<br />

<strong>Coating</strong>s in the Al-Ge-N system have been synthesized using reactive DC<br />

magnetron sputtering and characterized with the goal to explore the<br />

structure and properties, as well as their potential use as hard optical<br />

coatings. The composition was varied from pure AlN to pure GeNy. Also<br />

experiments varying substrate temperature and sample bias were conducted.<br />

<strong>Coating</strong>s were analyzed using X-ray diffraction, X-ray photoelectron<br />

spectroscopy (XPS) and scanning and transmission electron microscopy.<br />

Besides the binary reference samples, ternary samples with Ge-contents<br />

from 5 to 30 at.% were synthesized, and found to be nanocomposites of a<br />

nanocrystalline, Ge-containing AlN-phase, nc-(Al1-xGex)N, and an<br />

amorphous, N-deficient GeNy-phase. The grain size of the (Al1-xGex)N<br />

phase decreased with increasing Ge-content from about 30 to 15nm.<br />

Additionally the (Al1-xGex)N -phase was found to exhibit two different<br />

textures depending on the Ge-content: at low Ge content a (001) preferred<br />

orientation was observed, while at increased Ge-content the (110)<br />

orientation became dominant. The GeNy phase was found to be highly<br />

susceptible to sputter damage during sputter-cleaning prior to XPS analysis.<br />

A nanocomposite-hardening, similar to what has been observed for e.g. the<br />

AlN/Si3N4 system, was observed: the hardness increased from 19 GPa (for<br />

the AlN reference sample) to 25 GPa for the hardest ternary sample.<br />

Samples were found to have a high transparency in the visible region, and<br />

the index of refraction shows a slight dependence of Ge-content, increasing<br />

from about 2.0 to 2.2 as Ge-content increases from 0 to 30 at.%. Thus these<br />

coatings have a potential use as protective coatings for optical components<br />

operating in the visual or near IR range.<br />

3:50pm B5-2-7 Shape- Recovery of Thin Film Metallic Glasses Upon<br />

Annealing, C. Rullyani, C. Li, J. Chu (jpchu@mail.ntust.edu.tw), National<br />

Taiwan University of Science and Technology, Taiwan<br />

Thin film metallic glasses (TFMGs) possess many excellent and unique<br />

properties, including high strength, ductility, annealing-induced<br />

amorphization and good adhesion between the substrate and film. Like<br />

ordinary metallic glasses, the TFMGs in general undergo the glass transition<br />

and crystallization at temperatures of Tg and Tx, respectively, upon<br />

annealing. Another exceptional property of TFMGs is the shape-recovery<br />

ability during annealing at temperatures between Tg and Tx (or so-called the<br />

supercooled liquid region, ΔT) due mainly to the low viscosity flow.<br />

Surface defects such as indentation marks on the scales up to a few<br />

micrometers tend to shrink in size or even disappear without crystallization<br />

in ΔT.<br />

In this study, 200 nm-thick TFMGs with different compositions are<br />

deposited on Si substrates. Nanoindentation tests are performed to evaluate<br />

the film properties. Surface morphology and microstructure before and after<br />

annealing within ΔT are examined and reveal that the size of indentation<br />

mark decreases after annealing. As a result, the shape-recovery behavior is<br />

confirmed and detailed characterization results of various TFMGs as a<br />

function of annealing time will be discussed.<br />

Keyword: thin film metallic glass, annealing, shape recovery<br />

4:10pm B5-2-8 Thin Film Metallic Glasses: Unique Properties and<br />

Potential <strong>Application</strong>s, J. Chu (jpchu@mail.ntust.edu.tw), National<br />

Taiwan University of Science and Technology, Taiwan INVITED<br />

A new group of thin film metallic glasses (TFMGs) have been reported to<br />

exhibit properties different from conventional crystalline metal films,<br />

though their bulk forms are already well-known for the high strength and<br />

toughness, large elastic limits, excellent corrosion and wear resistances<br />

because of the amorphous structure. In recent decades, bulk metallic glasses<br />

(BMGs) have gained a great deal of interest due to the substantial<br />

improvements in specimen sizes. On the other hand, much less attention has<br />

been devoted to the TFMGs, despite the fact that they have many properties<br />

and characteristics which are not readily achievable with other types of<br />

metallic or oxide films. Furthermore, these TFMGs have been progressively<br />

used for engineering applications and thus deserve to be recognized in the<br />

field of thin film coatings.<br />

In addition, while the BMGs are still difficult to use because of their brittle<br />

macroscopic nature and difficulty of processing, TFMGs are a possible<br />

solution to make use of their great properties of high strength, large<br />

plasticity, and excellent wear resistance. In this presentation, many<br />

advantages and properties of TFMGs are discussed. These are such as<br />

mechanical properties, tribological properties, annealing-induced<br />

amorphization and resulting smooth surface, some of which lead to useful<br />

applications, for example, for substrate fatigue property enhancements. In<br />

addition, potential applications in microelectronics and optoelectronics are<br />

mentioned. Ironically, there have been enormous research efforts dedicated<br />

to developing metallic glasses with large critical sizes only to reveal that the<br />

best use for these materials may, in fact, be in thin film applications. It is<br />

thus hoped that this talk serves the purpose of calling attention to the<br />

importance of TFMGs such that many more studies and applications may be<br />

explored.<br />

4:50pm B5-2-10 Improving the corrosion resistance and hardness of<br />

TaN films by silicon addition, G. Ramírez (enggiova@hotmail.com), S.E.<br />

Rodil, S. Muhl, G. Galicia, Universidad Nacional Autónoma de México -<br />

Instituto de Investigaciones en Materiales, Mexico, E. Camps, L. Escobar-<br />

Alarcón, Instituto Nacional de Investigaciones Nucleares de México,<br />

México, D. Solis-Casados, Universidad Autónoma del Estado de México -<br />

Centro de Investigación en Química Sustentable, Mexico<br />

The aim of the present work was to obtain dense thin films that present<br />

simultaneously good corrosion resistance and hardness. For this, we<br />

propose the deposition of nanocomposite thin films where tantalum nitride<br />

(TaN) nanocrystals were embedded in an amorphous silicon nitride (SiNx)<br />

phase. The deposition was done using two magnetrons; one of pure Si and<br />

the other of pure Ta and the amount of Si into the samples was varied by<br />

changing the RF power (20 - 340 W) applied to the Si target. The N2/Ar<br />

ratio was fixed at the value optimized for the stoichiometric deposition of<br />

tantalum nitride films (6/14). The TaN-SiNx samples were deposited on<br />

silicon and their composition, structure and hardness were evaluated by Xray<br />

photoelectron spectroscopy, X.ray diffraction and nanoindentation,<br />

respectively. The results indicated that the silicon content increased linearly<br />

from 1 to 12 at% as the RF power was increased. Meanwhile, the hardness<br />

showed a maximum around 5.4 at% of silicon attaining 40 GPa,<br />

representing a 20 % hardness enhancement in comparison to the fcc phase<br />

of the TaN film. From the structural analysis, it was observed that the TaN<br />

d -fcc phase was stabilized due to the addition of Si. However, for the<br />

65 Wednesday Afternoon, April 25, <strong>2012</strong>

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