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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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3:10pm B1-2-6 The influence of deposited surface structures on<br />

mechanical properties, M.C. Fuchs (marcus.fuchs@s2003.tuchemnitz.de),<br />

N. Schwarzer, Saxonian Institute of Surface Mechanics,<br />

Germany<br />

It is well known and logical that certain deposition parameters have a great<br />

effect on surface structures like surface roughness, interface roughness,<br />

porosity, intergrain interaction, homogeneity or grain size. However, it is<br />

almost impossible to find deposition parameters or even ranges of them for<br />

processing of specific surface structures which are generally valid for all<br />

deposition techniques as there is a broad variety of them. Even with the<br />

same deposition technique only slight changes in the geometry of the<br />

deposition configuration can cause big differences. But such surface<br />

structures can influence the apparent mechanical properties of surface<br />

materials due to the method which is usually applied for determining them.<br />

Preferably one uses contact experiments like load-displacement sensing<br />

indentation measurements with subsequent classic Oliver & Pharr analysis,<br />

scratch or highly sophisticated (physicalized [1]) tribological tests.<br />

Consequently, deposition parameters can effect the resulting mechanical<br />

material properties like yield strength Y, hardness H and elastic modulus E.<br />

Such effects should be taken into account during the parameter<br />

identification analyzes of mechanical material properties. Because they are<br />

not only important for quantification of the mechanical behavior of<br />

coatings, but also important indicators (e.g. H in relation to E) for the<br />

tribological performance (e.g. wear, friction) of tribological coatings.<br />

Nevertheless, it is not possible to derive such effects on the mechanical<br />

material properties solely from the deposition parameters as a result of the<br />

dynamic nature of any deposition process. Hence, it is very important to<br />

know the resulting coating structure of a deposition process. It should be<br />

measured after processing when the surface is in a static state. Such effects<br />

and their partially dramatic influence on the resulting mechanical properties<br />

will be demonstrated on the examples of ta-C and nano-composite coatings.<br />

For example it will be shown how simple roughness can lead to false<br />

apparent ultra-hardness results. In the same context it is demonstrated how<br />

inadequate or incomplete analyzes features and theoretical approaches can<br />

directly lead to severely flawed conclusion about the actual coatings<br />

stability and reliability. Last but not least, of course, it will be shown how it<br />

is been done correctly.<br />

[1] Schwarzer et al.: “Optimization of the Scratch Test for Specific <strong>Coating</strong><br />

Designs”. SCT, accepted 2011.<br />

3:30pm B1-2-7 High Rate Magnetron Sputtering of Chromium<br />

<strong>Coating</strong>s for Tribological <strong>Application</strong>s, K. Nygren<br />

(kristian.nygren@mkem.uu.se), Uppsala University, Angstrom <strong>Lab</strong>oratory,<br />

Sweden, M. Samuelsson, Linköping University, Sweden, Å. Kassman-<br />

Rudolphi, Uppsala University, Angstrom <strong>Lab</strong>oratory, Sweden, U.<br />

Helmersson, Linköping University, Sweden, U. Jansson, Uppsala<br />

University, Angstrom <strong>Lab</strong>oratory, Sweden<br />

Increasing demands on tribological performance drive the development of<br />

innovative coating materials and deposition methods. Recent studies of<br />

reactively sputtered chromium carbide films show promising results with<br />

regards to coefficients of friction [1], and these coatings may be suitable for<br />

commercial purposes. However, transfer of a process to industrial<br />

conditions poses challenges, such as growing the films at significantly<br />

higher deposition rates. While this is known to influence the microstructure<br />

and phase content, which in turn determine the tribological performance,<br />

the implications for the Cr-C system are not fully understood.<br />

The objective of the present study is to investigate chromium carbide films<br />

deposited by direct current magnetron sputtering (DCMS) and high power<br />

impulse magnetron sputtering (HiPIMS) in an industrial deposition system,<br />

at growth rates up to 500 nm/min. While DCMS offers a higher deposition<br />

rate, HiPIMS is known to result in well-adherent, dense, and smooth<br />

coatings. Microstructural changes are expected as well as modified<br />

tribological and mechanical properties owing to the high deposition rate.<br />

Cr-C coatings were synthesized by sputtering of a Cr target in an Ar/C2H2<br />

atmosphere. XRD shows an X-ray amorphous Cr-C phase, in contrast to the<br />

nanocrystalline structure usually reported [2-3]. For DC sputtered coatings,<br />

XPS reveals a C-C phase which increases according to the phase diagram<br />

for Cr-C. The coatings produced by HiPIMS feature a meta-stable,<br />

supersaturated Cr-C phase, with a higher C content than predicted for the<br />

thermodynamically stable phase Cr3C2. Coefficients of friction were<br />

obtained from dry-sliding experiments (typically 0.35 – 0.50 for 34 – 0 %<br />

C-C), and the values confirm a dependence on phase fractions of C-C and<br />

C-Cr. Regarding the mechanical properties, coatings deposited by DCMS<br />

have a hardness of 14±1 to 18±1 GPa (51 to 17 at.% C), while coatings<br />

deposited by HiPIMS have a hardness of 7±3 GPa to 14±4 GPa (59 to 26<br />

at.% C). Unexpectedly, the coatings deposited by HiPIMS are softer than<br />

the ones deposited by DCMS, and this difference may be due to a different<br />

grain size or phase content. SEM cross-sections indicate deep Cr<br />

implantation in the substrate, which is known to improve adhesion. Further<br />

Monday Afternoon, April 23, <strong>2012</strong> 10<br />

results will be presented for a wide compositional range, and compared to<br />

literature.<br />

References<br />

[1] Mitterer et al, Proc IME J J Eng Tribol, 223 (2009) 751-757<br />

[2] Gassner et al, Tribol Lett, 27 (2007) 97-104<br />

[3] Agarwal et al, Thin Solid Films, 169 (1989) 281-288<br />

3:50pm B1-2-8 Behavior of DLC Coated Low-Alloy Steel under Tribo-<br />

Corrosion: Effect of Top Layer and Interlayer Variation, K. Bobzin, N.<br />

Bagcivan, S. Theiss, R. Weiß (weiss@iot.rwth-aachen.de), Surface<br />

Engineering Institute - RWTH Aachen University, Germany, U. Depner, T.<br />

Troßmann, J. Ellermeier, M. Oechsner, Institute for Materials Technology -<br />

TU Darmstadt, Germany<br />

In many industrial applications components are subjected to mechanical<br />

load, while being exposed to corrosive environments. In order to cope with<br />

the resulting tribo-corrosion, both corrosion and wear resistant steels are<br />

often resorted to. Since those materials are expensive and often difficult to<br />

machine, the development of protective thin films deposited on less<br />

expensive and easily machinable materials, is of high interest. Due to their<br />

chemical stability and high tightness, diamond-like carbon (DLC) coatings<br />

deposited via physical vapor deposition (PVD) seem to be appropriate to<br />

offer corrosion protection in addition to their well-established wear<br />

resistance. This paper deals with the development of DLC multilayer<br />

coatings consisting of alternating a-C and chromium based layers and an<br />

a-C:H top layer. The coatings were deposited on low-alloy steel (AISI<br />

4140) using reactive magnetron sputter ion plating (MSIP) technology to<br />

investigate the possibility of improving the properties concerning tribocorrosion.<br />

The mechanical and tribological properties of the top layer were<br />

analyzed depending on the ethine gas flow. Furthermore, the influence of<br />

different transitions from the a-C to the chromium based layers on the<br />

fatigue strength was investigated. The applicability of the DLC coatings in<br />

corrosive environments was proved using potentiodynamic polarization<br />

tests in artificial seawater: While the open circuit potential increases<br />

significantly from -400 mVH (AISI 4140) to about 300 mVH, current density<br />

remains below 0,001 mAcm -2 up to the maximum load of 1200 mVH (AISI<br />

4140: 100 mAcm -2 ). The tribological analyses regarding continuous sliding<br />

abrasion using a pin-on-disk tribometer show that the developed DLC<br />

coatings lead to very low wear rates in aqueous environment and in contact<br />

with an Al2O3 counterpart, nearly independent of the ethine gas flow.<br />

Moreover, investigations in an impact tribometer with maximum initial<br />

Hertzian stress of about 10 GPa show that pure metallic chromium layers<br />

with a soft transition to the a-C layers improve the fatigue strength of the<br />

compound. Thus, even after 10 6 impacts the coatings were proved to be still<br />

impenetrable for an electrolyte that could lead to corrosion of the substrate.<br />

4:10pm B1-2-9 Integration of the Larco ® -technology for ta-C-coatings<br />

in an industrial hard material batch system, M. Holzherr<br />

(katrin.wagner@vtd.de), M. Falz, T. Schmidt, VTD Vakuumtechnik<br />

Dresden GmbH, Germany, H.-J. Scheibe, M. Leonhardt, C.-F. Meyer,<br />

Fraunhofer-Institut für Werkstoff- und Strahltechnik, IWS, Germany<br />

DLC (diamond like carbon) thin film depositions are carried out in a wide<br />

range of CVD- and PVD technologies. Main applications are: tribologically<br />

stressed machine components as well as wear protection of tools. As a<br />

matter of fact, it could be verified that the hydrogen free DLC-coatings<br />

result in advanced thin film properties such as higher hardness which is<br />

caused by a higher sp 3 -bonding content. Therefore evaporation of solid<br />

graphite by PVD-technologies has been of considerable advantages.<br />

Especially the vacuum arc evaporation technique stands out for a very high<br />

degree of single and multiple ionised carbon atoms with increased energy<br />

necessary for condensation in the dense tetragonal amorphous diamondlike<br />

carbon film structure (ta-C). Beside low friction also super hard<br />

coatings can be deposited by means of that technology.<br />

A commercial hard material coating system has been equipped with a laser<br />

arc module (LAM) for the deposition of hydrogen-free ta-C-films. For<br />

industrial applications it was necessary to increase deposition rates.<br />

Therefore arc pulse current and pulse frequency were varied form 800 A to<br />

1.600 A and 150 Hz to 300 Hz, respectively.<br />

The carbon plasma during deposition process were examined by optical<br />

emission spectroscopy (OES) and Langmuir probe and effect on plasma<br />

parameters of the thin film properties will be shown.<br />

The influence of the deposition rate on thin film properties is caused by<br />

thermal effects. One limitation is a maximal deposition temperature of<br />

about 150 °C in order to avoid the graphite film structure which results in<br />

reduction of hardness finally.<br />

The thin film depositions were carried out on samples of circular blanks and<br />

carbide drills. Hardness, adhesion and elastic force module are the first<br />

criteria for evaluating the quality of the deposited ta-C- films. As real

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