ICMCTF1998 Session E5/D4-2: Properties & Applications of Diamond, Diamondlike and c-BN Coatings (2)

Thursday, April 30, 1998 1:30 PM in Room California

Thursday Afternoon

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1:30 PM E5/D4-2-1 Tribological Properties of Carbon Nitride Coating by Ion Beam Assisted Deposition
N. Umehara, K. Kato, T. Sato (School of Engineering, Tohoku University, Japan)

CNx coating is expected as hard overcoat of magnetic rigi d disk with long life. In this research, carbon sputtering and Nitrogen ion implantation were done simultaneously for production of carbon nitride as io n beam assisted deposition. After producing several coating of carbon includ ing nitrogen, their tribological properties were investigated. Substrate was silicon wafer disks with the diameter of 50mm and the thickness of 0.07Μm . After Ar ion bombardment for cleaning disk, Ar ion beam sputtering of carb on and implantation of nitrogen ion by N ion beam were done simultaneously. The acceleration energy and electric current of N ion beam was 500 eV and 40 mA/cm2, respectively. The thickness of coating deposited was about 100nm. According to ESCA analysis, carbon nitride coating contained 90 at% car bon and 10 at% nitrogen. No oxygen was found in the bulk material of the coa ting. Pin-on-disk type friction test was conducted for carbon nitride coating against,Si3N4 ball. During friction, surface temperature was controlled within the range from 20°C to 270°C by the electric heater from the back side of the substrate. Normal load and sliding speed we re 10 mN and 0.007m/s, respectively.

Surface temperature is high er than 18°C, friction coefficient gradually decreased with sliding distance and reached to a certain stable value. The relationship between the reached values of friction coefficient and surface temperature was investiga ted. Friction coefficient decreased with surface temperature of substrate. At surface temperature of 270°C, 0.026 of friction coefficient was obtained. > Regarding on wear property, no wear scar was observed with > optical microscope. Secondly, the effect of atmospheric air > on friction coefficient was investigated. in only high > vacuum, low friction was observed at high tem perature.

1:50 PM E5/D4-2-2 Friction Mechanism of Diamond-like Carbon: Effect of Gas and Temperature
C. Donnet, T. Le Mogne, L. Ponsonnet, M. Belin (École Centrale de Lyon, France); A. Grill, V. Patel, C. Jahnes (T.J. Watson Research Center)
The present study proposes to discuss the influence of the gaseous environment and temperature on the friction behavior of diamond-like carbon coatings. Using a dedicated UHV tribometer, reciprocating pin-on-flat friction tests have been performed on hydrogenated DLC films at various partial pressures of pure oxygen or pure water vapor, and in ultrahigh vacuum, in the temperature range 20 - 550°C. The maximum gaseous pressures of oxygen and water vapor were respectively 60 hPa and25 hPa, the second value corresponding to a relative humidity RH = 100% at room temperature. It was found that, in the investigated pressure range, oxygen has no influence on the ultralow friction behaviour observed in UHV. Conversely, water vapor, at pressures in the range of 0.1-1 hPa, drastically changes the friction behavior, increasing the friction from less than 0.02 to more than 0.1. Heat treatments performed in UHV before or during the tribological tests affect the friction behavior, depending on the nature of the film, in particular the relative fraction of hydrogen bounded to carbon. Chemical analysis performed by in situ Auger spectroscopy inside the wear tracks and by electron energy loss spectroscopy on wear particles, allowed to elucidat the friction mechanisms responsible for the tribological behaviors observed.
2:10 PM E5/D4-2-3 Tribological Fundamantals and Potential Applications of c-BN Films
S. Miyake, S. Watanabe, M. Murakawa (Nippon Institute of Technology, Japan)
Tribology is a key technology of modern tribo-elements used in the advanced industry. In this field, atomic-scale wear and friction fluctuations degrade equipment performances. New hard, lubricating coatings such as cubic BN film seem to be useful in reducing this wear and friction. This paper discusses a macro- and microtribological properties of cubic BN films that reduce wear and friction, and then discussed potential applications of these cubic BN films to modern tribo-elements such as high precise processing tools, micromachines, protective coatings used in file memories and sliding parts used in vacuum.
2:50 PM E5/D4-2-5 Fretting Wear Behavior of Diamondlike Carbon (DLC) Coated Ti-6Al-4V
B. Pohlchuck, K. Miyoshi (NASA Lewis Research Center); R.L.C. Wu (K Systems Corporation)
A fretting wear simulation rig using a pin on flat configuration has been developed and verified. Adjustable test parameters include the applied load, amplitude, frequency, and relative humidity. The rig was utilized to conduct fretting wear experiments with uncoated Ti-6Al-4V against itself under the following conditions: room temperature, 1.47N load, 75 micrometer amplitude, 80Hz frequency, and <1%-100% relative humidity. Wear was found to be significantly dependent on the ambient relative humidity up to 30%. From 30% to 100% relative humidity there was almost no change in the wear rate. Work currently being conducted with ion-beam-deposited DLC on Ti-6Al-4V in contact with uncoated Ti-6Al-4V will be presented, including a discussion of the dependency between amplitude and fretting wear. In these studies amplitude was varied between 5 to 50 micrometers and relative humidity held between 40% and 50%. Coating effectiveness will be determined by comparing the wear rate of DLC coatings to those previously obtained on uncoated Ti-6Al-4V.
3:30 PM E5/D4-2-7 Nanostructure and Photoconductivity Studies of a-DLC Films Deposited by RF Plasma
N. Croitoru, M. Maharizi, L. Klibanov, A. Seidman (Tel-Aviv University, Israel)

In this paper the optimum parameters of RF plasma deposition which enabled us to obtain DLC (Diamond Like Carbon) films with maximum ratio of the sp3/sp2 bondings, suitable for electron and photoelectron devices, were studied. A ailed study of the nano- and microstructure as a function of thickness was performed using AFM , STM and SEM , optical microscope, respectively. The deposited films were of thickness( 10 ≤ d ≤ 1000 nm). The results obtained from this study have s n that a mixture of microcrystalline (c) and amorphous (a) DLC and graphite (G) was deposited on the substrate. The ratio of c-(DLC/G) and of a-(DLC/G) is a function of the parameters of deposition (RF plasma power, CH4 pressure and type of substrate). man spectroscopy and microhardness investigation have given additional results which enabled us to obtain the conditions of deposition for which a maximum value of the ratio of diamond (sp3/) to graphite (sp2/) bondings.

Special attention was paid to the influence of the type of substrate on the composition of the DLC films. Deposition on silicon and germanium single crystals, sapphire, Corning glass, and alumina were made. Substrates of average roughness less than 10 was observed, which are suitable for growing homogeneous amorphous films. Scratches or other defects on the substrates (e.g. sapphire) act as centers of crystallization. Images of AFM have shown the mechanism of increase of the DLC layers on the surfac f substrate between scratches.

Doping with iodine (I2) was made by deposition the of the films from a mixture of CH4 + 20 % I2 . Measurements of dark and photocurrent have shown that I2 compensates the "dangling bonds" of the DLC films due to the disorder structur The decrease of dangling bonds which act as traps or recombination energetic levels, increased the life time of injected free carriers under light and the value of concentration of I2 for which photocurrent appears at room temperature was determi .

3:50 PM E5/D4-2-8 Auto-lubrication of Diamond Coatings at High Sliding Speed
T. Le Huu, D. Paulmier (National Polytechnics Institute of Lorraine, France); A. Grabcheko (Kharkov State Polytechnical University, Ukraine); M. Horvath, I. Mészaros (Technical University of Budapest, Hungary); A.G. Mamalis (National Technical University of Athens, Greece)

We investigated the friction and wear properties of diamond coatings at high sliding speed (V=35 m/s).

Various types of diamond coatings were deposited on tungsten carbide pins.

These coatings are produced by combustion flame method under different deposition conditions.

The surface properties and morphology of the coatings have been characterised by surface analysis methods such as Scanning Electron Microscopy (SEM), and Raman Spectrometry (RS).

The coated pins slide against a steel XC30 rotating disc in ambient atmosphere.

The hardness of coated pin is 70 GPa and this one of disc after heat treatment is 5 GPa.

The experimental results show that at low sliding speed (V=1m/s) the diamond coatings exhibit very high friction coefficient, μ is about 0.8 to 1.

At high sliding speed (V=35 m/s) the friction coefficient of these films decreases to μ = 0.09 - 0.15, the wear of the diamond films was also decreased.

This tribological behaviour of diamond coatings can be explained by the transformation of sp3 to sp2 carbon sites on the rubbing surface during friction at high sliding speed, inducing their reconstruction or creation on them of double (π sp2) bonds.

A model of the friction is presented to explain this phenomenon.

4:10 PM E5/D4-2-9 Industrial Applications of Diamond Coated Cutting Tools with Adapted Surface Morphologies Coated in an Innovative Hot-Filament Production Unit
O. Lemmer, T. Leyendecker, St. Esser, M. Frank, R. Lammers (CemeCon GmbH, Germany)
Excellent lifetimes are achieved in machining workpiece materials like reinforced plastics, presintered ceramic compacts, aluminum and magnesium alloys, metal-matrix composites, graphite as well as other high-tech materials by using CVD-diamond coated cutting tools. It is shown that the performance of these tools can exceed even expensive conventional PCD. These superior wear properties of diamond can only come into action, if the surface morphology of the diamond coating is adapted to the specific conditions. Using an innovative hot-filament production unit, the microscopic structure can be determined by in-situ methods and can replace ex-situ methods like grinding or laser ablation. Since many investigations exist for microwave CVD on silicon, here is shown how adapted surface morphology can be perfectly achieved by methods based on the hot filament technique. These methods work excellently even on technical substrates as cemented carbides and silicon nitride as well as on complex tool geometries.
4:30 PM E5/D4-2-10 A Study of the Tribological Properties of Thick Sputtered Carbon Films.
D. Camino, A.H.S Jones, D.G Teer (Teer Coatings Ltd, England)

Sputtered carbon films deposited by closed field unbalanced magnetron sputter ion plating up to 1 micrometer thick have shown improved tribological properties[1]. When the film thickness was increased the films’ performance in mechanical wear tests was reduced. This was thought to be a result of increased internal stresses within the film.

In order to produce low friction, wear resistant films of thicknesses greater than 1micrometer, the inclusion of oxygen, nitrogen and co-sputtered metal in the carbon films has been studied. Deposition parameters have been optimised to improve the performance in tribological tests in air, oil and water. The films have been characterised using micro hardness testing, pin on disc and reciprocating friction and wear tests and the results are presented. The structure of the coatings has been studied by optical microscopy and SEM of normal and taper sections produced by ball cratering techniques.

References.

[1]. ‘Novel DLC Coatings Deposited by Magnetron Sputtering of Carbon Targets’ D.G. Teer, A.H.S. Jones, V. Bellido Gonzalez, D. Camino. Metallurgical Coatings and Thin Films 1997, Proceedings of the 23rd International Conference on Metallurgical Coatings and Thin Films, San Diego, CA, USA, April 1997.

4:50 PM E5/D4-2-11 Cylindrical CVD Diamond for High Performance Small Abrading Devices
V.J. Trava-Airoldi, J.R. Moro, E.J. Corat, E.C. Goulart, S. Silva, N.F. Leite (Universidade de São Francisco, Brazil)
Columnar grain structure studies have been carried out on small curvature radio cylinder substrate in developing small abrading devices. An enhanced hot filament assisted technique was used. The substrate holder have a movable mechanism magnetically coupled to a DC motor placed outside of the reactor chamber. Free standing diamond film as thick as 1 mm were obtained on molybdenum wire substrates. The substrates varied from 150 up to 1200 micrometer diameter and were as long as 50 mm. A relationship of the curvature radius of the substrate surface with the growth rate and the spread of the column volume have been observed. A preferential diamond (111) surface morphology have been obtained which is strongly dependent on diamond growth parameters, including the substrate position and its angular velocity. The worst obstacle to obtain very high abrading surface was the renucleation process. Grain size up around 150 micrometer was obtained. In this work we also report an interesting application involving the characteristics of the (111) diamond surface as a small abrading device. Some results of cylindrical diamond burrs and diamond drills for non-ferrous wear are shown.
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