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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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eactive gases with the target material. So, investigation was carried out the<br />

effects of sputtering gases for the preparation of CNx films by RF reactive<br />

sputtering. CNx films were prepared using RF magnetron sputtering<br />

apparatus. Graphite was used as a target and Si was used as the substrate.<br />

The substrate was pretreated to immerse on BHF for 5 minutes. RF power<br />

and pressure were fixed to 200W and 0.4Pa, respectively. Ar and N2 were<br />

used as sputtering gases and their ratio was Ar/N2=1/0, 1/1, 1/3, and 1/5.<br />

The sputtering time was 60 minutes. The CNx films were prepared after<br />

pre-sputtering using same condition for 10 minutes. The deposits were<br />

estimated by using of SEM, XPS and Raman spectroscopy. From the crosssectional<br />

SEM images, deposition rate was increased by adding of N2 to Ar<br />

sputtering gas and floating substrate holder potential. As a result of Raman<br />

spectroscopy, the DLC broad peak center around 1550cm-1, D-band peak<br />

center around 1350cm-1, G-band peak center around 1580cm-1and S-band<br />

peak center around 1200cm-1 were observed in spectra of each samples. As<br />

a result of XPS, the peaks of C-C and -C=O bond were observed in C1s<br />

spectra of the deposit prepared using Ar. The peaks of C-C, C=O, N=O-, C-<br />

N, =C-N=C- and -C≡N bond were observed in C1s and N1s spectra used<br />

mixture of Ar and N2 as sputtering gases. As mention above, the deposit<br />

contain nitrogen was obtained using the mixture of Ar-N2 gases. As a result<br />

of preparation of CNx films by RF reactive sputtering, DLC was obtained<br />

using Ar as the sputtering gases. On the other hand, it was possible to<br />

prepare CNx using the mixture of Ar and N2 gases as a sputtering gas.<br />

9:00am B1-3-4 Zirconium carbonitrides: study of tribological<br />

properties with deposition parameters, J. Barriga<br />

(jbarriga@tekniker.es), L. Mendizabal, U. Ruiz de Gopegui, Tekniker,<br />

Spain<br />

In the last years a great effort has been done in the development of carbon<br />

based coatings for tribological applications. As a consequence, the sliprolling<br />

resistance of DLC thin films was improved considerably. On the<br />

other side, zirconium has been used widely in the decorative industry<br />

because of its corrosion resistance and wide range of affordable metallic<br />

colors. But the use of Zr in tribological thin films is not very broad.<br />

However, recent developments show that zirconium based coatings could<br />

perform better than DLC thin films in tribological contacts under severe<br />

contact conditions [1].<br />

In the present work, zirconium carbonitride thin films have been developed<br />

on M2 steel by cathodic arc evaporation under a wide range of deposition<br />

parameters. BIAS voltage has been varied from 30 to 400 V. Temperature<br />

during the process has also been controlled from 500ºC to 300ºC, in order to<br />

study the possibility of doing the deposition at low temperatures opening<br />

the range of substrate steels. Finally, the flux of acetylene gas has also been<br />

varied to study the influence of carbon content in the properties of the film.<br />

A wide characterization procedure has been taken with the resulting ZrCN<br />

coatings: Calotest, SEM, X-Ray analysis, adhesion tests and, finally, a<br />

battery of sliding tribological tests. With this we have analyzed the<br />

influence of deposition parameters on the films and looking for the proper<br />

applications of the best performing films.<br />

[1] Charles-Alix Manier, Holger Ziegele, Javier Barriga, Josu Goikoetxea,<br />

Mathias Woydt, Zirconium-based coatings in highly stressed rolling<br />

contacts as alternative solution to DLC and ta-C coatings, Wear 269 (2010)<br />

770–781.<br />

9:20am B1-3-5 Comparison of sputter deposited WC coatings from<br />

alternative sources, H. Alagoz (alagoz@bilkent.edu.tr), E. Uzun, M.<br />

Ugras, N. Uddin, E. Bengu, Bilkent University, Turkey<br />

Transition metal nitride and carbide coatings attracted a lot of attention in<br />

the last decades due to their good wear, erosion, corrosion and high<br />

temperature oxidation resistance. In this study, an alternative synthesis<br />

approach was used for the synthesis of carbide coatings in the W-C system.<br />

New WxCy coatings were synthesized by reactive magnetron sputtering<br />

technique with various target combinations and gas compositions on<br />

Si(100) and steel (100Cr6) substrates. Instead of the frequently used carbon<br />

sources such as WC(1:1) or graphite target, and CH4 or C2H2 gases, a B4C<br />

target was used as an alternative for C source and N2 gas was fed through<br />

the chamber during deposition. For comparison, another set of coatings<br />

were synthesized using an additional graphite target together with allowing<br />

C2H2 gas feed instead of N2 flow in order to see the effect of increasing C<br />

content in the coatings. We investigated the change in the phase<br />

composition, chemical bonding, hardness, room-temperature and hightemperature<br />

wear rates of these two sets of coatings. Scanning electron<br />

microscopy (SEM) was used to understand the effect of process parameters<br />

on surface roughness and microstructure of the films. The hardness values<br />

of the films were measured using the nano-indentation technique and, we<br />

used a high-temperature tribometer (up to 800°C) to investigate the wearrates<br />

of the coatings. X-ray photo-electron spectroscopy (XPS) has been<br />

employed to understand the bonding states of tungsten and carbon as well<br />

as boron, nitrogen and oxygen on the as-deposited surfaces. Our results<br />

showed that the coatings are mostly combinations of W+WC, W+W2C and<br />

BN in the case of N2 flow. <strong>Coating</strong>s containing BN species are showing<br />

considerably good hardness (up to 31.5 GPa) and wear performances(up to<br />

2.0x10 -7 mm 3 /Nm at room-temperature and 2.0x10 -6 mm 3 /Nm at 500 o C).<br />

Increasing the C content of the films in the second set of experiments did<br />

not cause a significant change on the wear rates but gave a gradual decrease<br />

to the hardness and friction coefficient of the films.<br />

9:40am B1-3-6 The influence of the magnetic field strength on the<br />

poisoning behavior of Tantalum, R. Hollerweger<br />

(robert.hollerweger@unileoben.ac.at), Montanuniversität Leoben, Austria,<br />

M. Lechthaler, OC Oerlikon Balzers AG, Liechtenstein, P. Polcik,<br />

PLANSEE Composite Materials GmbH, Germany, J. Paulitsch, P.H.<br />

Mayrhofer, Montanuniversität Leoben, Austria<br />

Reactive magnetron sputtering requires precise knowledge of the chemical<br />

and physical processes in the plasma itself as well as at the target surface.<br />

Therefore, a lot of investigations are focusing on the poisoning behavior in<br />

dependency of parameters like power density, reactive gas partial pressure,<br />

total pressure or magnetic field configuration. Especially the change of the<br />

magnetic field strength due to progressing target erosion has a pronounced<br />

influence on the target poisoning as well as plasma conditions and hence, on<br />

the plasma and film properties. To investigate this effect, voltage hysteresis<br />

curves were recorded while sputtering a Ta target in Ar-O2 atmosphere. The<br />

magnetic field strengths and DC current densities were subsequently varied<br />

from 45 to 90 mT and from 13 to 26 mA/cm², respectively. Due to these<br />

variations, a shift of the different sputtering regimes within the hysteresis<br />

can be detected. Selected points, referring to oxygen gas contents of 42, 70<br />

and 100 % of the total gas flow, were used for the deposition and<br />

characterization of Ta2O5 thin films, which indicate hardness values in the<br />

range of 15 GPa, crystalline structure and high thermal stability. This<br />

comprehensive study of the sputtering behavior helped to gain well-founded<br />

knowledge of possible influences on the poisoning behavior of Tantalum as<br />

well as on the film formation processes of the resulting pentoxide.<br />

10:00am B1-3-8 Cavitation and abrasion resistance of Ti-Al-Y-N<br />

coatings prepared by the PIII&D technique from filtered vacuum-arc<br />

plasma, V. Belous, V. Vasyliev, A. Luchaninov, V. Marinin, E. Reshetnyak,<br />

V. Strel’nitskij, National Science Center “Kharkov Institute of Physics and<br />

Technology”, Ukraine, S. Goltvyanytsya, V. Goltvyanytsya<br />

(vladtnt@gmail.com), Real Ltd., Ukraine<br />

Ti-Al-Y-N coatings with small Y percentage have demonstrated high<br />

hardness and excellent oxidation resistance which provides their application<br />

for protection the machine parts which operate under extreme<br />

environmental conditions. In our recent work [1] we investigated structure<br />

and properties of such coatings prepared by the plasma immersion ion<br />

implantation and deposition (PIII&D) using filtered vacuum-arc plasma<br />

source.<br />

Deposition from the filtered vacuum arc plasma is the widely used effective<br />

method of manufacturing high quality protective wear resistant coatings. A<br />

high-voltage pulsed bias applied to the substrate permits the deposition of<br />

thicker coatings with good adhesion and low residual stresses. In the present<br />

work we examined the cavitation and abrasion resistance of PIII&D<br />

deposited Ti-Al-Y-N coatings doped with yttrium (≤ 1 at.%) and analyzed<br />

correlation between their properties and structure.<br />

Ti-Al-Y-N coatings with thickness of 5-6 micron were deposited on the 302<br />

stainless steel substrates from filtered vacuum-arc plasma at nitrogen<br />

pressure of 0.1 Pa. Ti0.5-xAl0.5Yx alloys (x = 0, 0.002, 0.004 and 0.01)<br />

produced by vacuum-arc remelting in argon atmosphere (by Real Ltd.,<br />

Zaporozhye, Ukraine) were used as cathodes in the vacuum-arc plasma<br />

source. The substrate potential was either DC (-150 V) or negative pulsed,<br />

the amplitude AU varied in the range of 0-2.5 kV.<br />

The erosion resistance of the coatings was evaluated on the measured mass<br />

loss during cavitation treatment in distilled water. The tests were continued<br />

until visually watched open-ended pores in the coating were formed.<br />

Abrasion wear was determined in the scheme substrate plane – rotating<br />

abrasion disk.<br />

The substrate potential during deposition process and Y content in the<br />

coatings were found to be important factors influencing the rate and<br />

character of their cavitation damage. The coating deposited at AU=0 was<br />

subjected to pitting erosion. Long cracks prevailed on the surface of the<br />

cavitation treated coating deposited at DC (-150 V) potential. High voltage<br />

pulsed substrate potential contributed to decrease by 3-5 times in the rate of<br />

the mass loss under cavitation, quantity of the erosion defects on the treated<br />

surface diminishes sharply. Increase of Y content resulted in improvement<br />

of wear durability. Mean rates of cavitation and abrasion wear of<br />

(Ti,Al)N+1at.%Y were a factor of 3 to 5 times lower than that of (Ti,Al)N<br />

and tenfold lower than that of TiN.<br />

25 Tuesday Morning, April 24, <strong>2012</strong>

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