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Sputtering technology in solid film lubrication

Current and potential sputtering technology is reviewed as it applies primarily to the deposition of MoS2, though such lubricants as WS2 and PTFE are also considered. It is shown by electron microscopy and surface sensitive analytical techniques that the lubricating properties of sputtered MoS2 films are directly influenced by the sputtering parameters selected (i.e., power density, pressure, sputter etching, dc-biasing, etc.), substrate temperature, chemistry, topography, and environmental conditions during the friction test. Electron micrographs and diffractograms of sputtered MoS2 films clearly show the resultant changes in film morphology which affect film adherence and frictional properties.

Spalvins, T.

Simultaneous ion sputter polishing and deposition

Results of experiments to study ion beam sputter polishing in conjunction with simultaneous deposition as a mean of polishing copper surfaces are presented. Two types of simultaneous ion sputter polishing and deposition were used in these experiments. The first type utilized sputter polishing simultaneous with vapor deposition, and the second type utilized sputter polishing simultaneous with sputter deposition. The etch and deposition rates of both techniques were studied, as well as the surface morphology and surface roughness.

Rutledge, S.

Structural and compositional characterization of RF sputter-deposited Ni-Cr + Cr2O3 films

An RF-sputtered chrome oxide coating with metallic binders was developed. The chrome oxide coating has high-temperature capabilities and is wear resistant, and has some self-lubricating properties. A nichrome metallic binder was added in the coating to improve its ductility without significant loss in the hardness. The sputtering parameters were optimized to obtain a smooth coating with the maximum adherence. The coatings were applied using bias-sputter and sputter-deposit modes on the heat treated and annealed foil substrates. The coating applied on annealed foils using the sputter-deposit mode was smooth and had the best adherence. Metallurgical examinations showed that the coating was Ni-Cr + Cr2O3. The coating as applied was amorphous and it crystallized during substrate heat treatment.

Bhushan, B.

Ion beam sputter deposited diamond like films

A single argon ion beam source was used to sputter deposit carbon films on fused silica, copper, and tantalum substrates under conditions of sputter deposition alone and sputter deposition combined with simultaneous argon ion bombardment. Simultaneously deposited and ion bombarded carbon films were prepared under conditions of carbon atom removal to arrival ratios of 0, 0.036, and 0.71. Deposition and etch rates were measured for films on fused silica substrates. Resulting characteristics of the deposited films are: electrical resistivity of densities of 2.1 gm/cu cm for sputter deposited films and 2.2 gm/cu cm for simultaneously sputter deposited and Ar ion bombarded films. For films approximately 1700 A thick deposited by either process and at 5550 A wavelength light the reflectance was 0.2, the absorptance was 0.7, the absorption coefficient was 67,000 cm to the -1 and the transmittance was 0.1.

Banks, B. A.

Sputtering phenomena in ion thrusters

Sputtering effects in discharge chambers of ion thrusters are lifetime limiting in basically two ways: (1) ion bombardment of critical thruster components at energies sufficient to cause sputtering removes significant quantities of material; enough to degrade operation through adverse dimensional changes or possibly lead to complete component failure, and (2) metals sputtered from these intensely bombarded components are deposited in other locations as thin films and subsequently flake or peel off; the flakes then lodge elsewhere in the discharge chamber with the possibility of providing conductive paths for short circuiting of thruster components such as the ion optics. This experimental work has concentrated in two areas. The first has been to operate thrusters for multi-hour periods and to observe and measure the films found inside the thruster. The second was to simulate the environment inside the discharge chamber of the thruster by means of a dual ion beam system. Here, films were sputter deposited in the presence of a second low energy bombarding beam to simulate film deposition on thruster interior surfaces that undergo simultaneous sputtering and deposition. Mo presents serious problems for use in a thruster as far as film deposition is concerned. Mo films were found to be in high stress, making them more likely to peel and flake.

Robinson, R. S.

Magnetron-Sputtered Amorphous Metallic Coatings

Amorphous coatings of refractory metal/metalloid-based alloys deposited by magnetron sputtering provide extraordinary hardness and wear resistance. Sputtering target fabricated by thoroughly mixing powders of tungsten, rhenium, and boron in stated proportions and pressing at 1,200 degrees C and 3,000 lb/in. to second power (21 MPa). Substrate lightly etched by sputtering before deposition, then maintained at bias of - 500 V during initial stages of film growth while target material sputtered onto it. Argon gas at pressure used as carrier gas for sputter deposition. Coatings dense, pinhole-free, extremely smooth, and significantly resistant to chemical corrosion in acidic and neutral aqueous environments.

Thakoor, A. P.

Nb3Sn Superconducting Radiofrequency Cavity Fabricated by Sputter Deposition from a Stoichiometric Target

Nb$_3$Sn is a promising coating material for superconducting radiofrequency cavities in next-generation accelerators due to its higher superconducting transition temperature (~18.3 K) and superheating field (~400 mT), offering the potential to surpass the intrinsic performance limits of bulk niobium. We developed a sputter coating technique employing a stoichiometric target to fabricate Nb$_3$Sn films on the inner surfaces of niobium cavities. A Nb$_3$Sn tube target, prepared by growing a >20 m thick Nb$_3$Sn coating on the surface of a Nb tube via a Sn vapor diffusion process, was used in a DC cylindrical magnetron sputtering system. Approximately 170 nm thick Nb-Sn films were sputter-coated onto flat Nb substrates positioned to replicate the beam tube and equator regions of a 2.6 GHz cavity, followed by annealing at 950 °C for 3 hours to form Nb$_3$Sn. The composition, morphology, and structure of the annealed Nb$_3$Sn films were examined. Then, a ~1.2 m-thick film was sputter-coated onto the interior of a 2.6 GHz Nb cavity following the procedure developed for the flat samples. The cavity was subsequently annealed under the same conditions used for the flat samples. Cryogenic RF testing of the sputter-coated cavity demonstrated a T$_c$ of approximately 17.8 K, consistent with Nb$_3$Sn layer. Subsequently, the cavity underwent a light Sn recoating followed by a vapor diffusion Nb$_3$Sn coating process, achieving a quality factor of approximately 8.5 × 10$^9$ and an accelerating gradient of up to 11.3 MV/m at 4.2 K.

Shakel, Md Sharifuzzaman [Old Dominion U.; Jeffers

Molecular dynamics simulations of reflection and sputtering behavior of boron under deuterium ion irradiation

Boronization is a commonly used method of wall conditioning in fusion reactors. The application of boron films to the plasma-facing materials results in enhanced plasma performance due to the reduction of intrinsic impurities. This is primarily driven by a reduction in oxygen content that is chemically trapped in the boron film. The reactive nature of these boron films also raises questions concerning interactions with hydrogen isotopes. In this work, boron-deuterium interactions were studied using molecular dynamics (MD). Reactive force field potentials were used to model the chemical interactions between B and D. An amorphous boron substrate was irradiated by D atoms at varying incident energies, 10 eV < E i < 150 eV and angles, 0° < α < 85°. The reflection probability was calculated and compared to results from the commonly-used binary collision approximation (BCA) method. This comparison found that the BCA underestimated the reflection probability at E i < 35 eV and α > 45 ∘ . The source of this discrepancy was found to be the surface binding energy model. The BCA calculation with an isotropic surface binding energy model was more closely aligned to the MD result. This, in combination with a correction function based on the MD results allows for corrections to the reflection probability of deuterium impinging on boron surfaces. The sputtering of the substrate material was also studied. While this study did not contain sufficient events to quantitatively describe the sputtering behavior, some qualitative results emerged: namely, chemical sputtering of B and D-containing molecules (BD, BD 2 , BD 3 ) at low ( < 20 eV) incident deuterium energies. This result suggests that chemical sputtering could be a significant factor in limiting boron coating lifetime when exposed to lower ion energies, such as those in detached plasmas. The results show that chemical interactions should be taken into account when modeling the interactions between D ions and B surfaces.

Boron

Net lithium deposition and dominant self-sputtering in lithium tokamak experiment-β with a liquid lithium wall

We observed enhanced net lithium deposition and lithium erosion, possibly dominated by physical sputtering of lithium by lithium-ion bombardment, on the outer plasma-facing surface in the Lithium Tokamak eXperiment-β (LTX-β) during liquid lithium wall operations. Silicon crystal samples with micro-trenches (30 μm × 30 μm × 2–7 μm deep) were exposed to hydrogen plasmas in LTX-β for solid and liquid lithium wall operations. Post-mortem analysis using X-ray photoelectron spectroscopy combined with argon ion sputtering measured net lithium deposition of 8.2 or 21 nm on the silicon crystal surface exposed for ~ 50 repeated shots of ~ 50-ms hydrogen plasma discharges during the liquid lithium wall operations at a vessel temperature of 475 K. Energy dispersive X-ray spectroscopy measured oxygen concentration patterns on the micro-trench floors, which were due to oxidized lithium deposition. Using the inhomogeneous oxygen concentration pattern caused by an ion-shadowing effect associated with the micro-trench’s geometric structure, we determined a polar incident ion direction of 68.4 ± 1.6° referenced to the surface normal direction. This observation was well-explained by the hypothesis that self-sputtering of Li was a dominant lithium erosion source in addition to lithium sputtering by hydrogen bombardment.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY

Radiofrequency-sputtered coatings for lubrication system components and other complex surfaces

Irregularly shaped surfaces, such as lubrication system components (ball bearings, seals, gears, etc.), can be coated on all surfaces, including irregular shapes, when radiofrequency sputtering is used. When the specimen is properly located with respect to the sputtering target, the sputtered material covers the entire surface of the object irrespective of its geometrical configuration. An adherent, dense film is formed. The film thickness varies from 20 to 50 percent on, for example, a hearing cage or race depending on its geometry. When sputtered solid film lubricants such as molybdenum disulfide are used, a film thickness only of the order of 10 to the minus 7th power m (thousands of angstroms) is required at the contacting areas. It is only essential to determine the required film thickness at the critical areas in need of lubrication. The sections outside the areas to be lubricated fall within the thickness deviation range of 20 to 50 percent, which still constitutes a negligible change respect to tolerance requirements.

Spalvins, T.

Sputtering and ion plating

The proceedings of a conference on sputtering and ion plating are presented. Subjects discussed are: (1) concepts and applications of ion plating, (2) sputtering for deposition of solid film lubricants, (3) commercial ion plating equipment, (4) industrial potential for ion plating and sputtering, and (5) fundamentals of RF and DC sputtering.

Source record

Change in transmittance of fused silica as a means of detecting material sputtered from components on a 5-cm ion thruster

Two endurance tests of a 5-cm mercury bombardment thruster are reported. Both tests used a translational screen-grid system with the beam vectored 10 degrees. The first test lasted 141 hours and the second test operated for 2026 hours. In each test two fused silica samples (solar cell covers), 2.0 cm by 2.1 cm, were placed in shielded holders to detect materials sputtered from the thruster. Spectral optical properties between 0.398 and 2.16 microns were measured on each sample, both before and after the endurance tests. The deposition on each sample was spectrographically analyzed to determine the type of materials sputtered from the thruster. It was found that sputtering from the neutralizer is highly dependent on its position with respect to the beam edge. The sputtering from the accelerator grid of the translational screen-grid system of the 2026 hour test was sufficient to form an opaque film on the sample located in the direction opposite to the vectored beam.

Weigand, A. J.

Structure of molybdenum disulfide films sputtered on substrates at various temperatures

Molybdenum disulfide films 300 to 400 A thick were rf sputtered on aluminum and nickel surfaces at elevated, ambient, and liquid nitrogen temperatures. Electron transmission micrographs and electron diffraction patterns were taken to determine the structural growth. These transmission micrographs revealed that sputtered MoS2 films at ambient and elevated temperatures (320 and 150 C) formed an irregular network of ridges. The electron diffraction patterns of these films showed relatively sharp diffraction rings, indicating crystallinity. The transmission micrographs of sputtered films at liquid nitrogen temperatures revealed a continuous featureless film. The electron diffraction patterns showed broad, diffused rings indicating an amorphous film. The transmission micrographs of a post-annealed (425 C) MoS2 film sputtered at liquid-nitrogen temperature revealed the tendency for ridge formation. Electron diffraction patterns also showed increased sharpness of the diffraction rings. Friction tests showed that MoS2 films deposited at ambient and elevated temperatures exhibited good lubricating properties. The MoS2 films deposited at cryogenic temperatures had no lubricating characteristics.

Spalvins, T.

On the sputtering of binary compounds

A simple physical model is presented to describe some aspects of the sputtering of compound targets. In particular, expressions are developed for the partial sputtering yields for binary systems in terms of the elemental sputtering rates, the stoichiometric concentrations and surface binding energy. The partial yields depend non-linearly on the bulk target concentrations. Comparison of the theoretical predictions with the data on sputtering of PtSi, NiSi and Cu3Au indicates that the general features are well described.

Haff, P. K.

Microstructural and wear properties of sputtered carbides and silicides

Sputtered Cr3C2, Cr3Si2, and MoSi2 wear-resistant films (0.05 to 3.5 microns thick) were deposited on metal and glass surfaces. Electron transmission, electron diffraction, and scanning electron microscopy were used to determine the microstructural appearance. Strong adherence was obtained with these sputtered films. Internal stresses and defect crystallographic growth structures of various configurations within the film have progressively more undesirable effects for film thicknesses greater than 1.5 microns. Sliding contact and rolling element bearing tests were performed with these sputtered films. Bearings sputtered with a duplex coating (0.1-micron-thick undercoating of Cr3Si2 and subsequently 0.6-micron coating of MoS2) produced marked improvement over straight MoS2 films.

Spalvins, T.

X-Ray photoelectron spectroscopy study of radiofrequency-sputtered titanium, carbide, molybdenum carbide, and titanium boride coatings and their friction properties

Radiofrequency sputtered coatings of titanium carbide, molybdenum carbide and titanium boride were tested as wear resistant coatings on stainless steel in a pin on disk apparatus. X-ray photoelectron spectroscopy (XPS) was used to analyze the sputtered films with regard to both bulk and interface composition in order to obtain maximum film performance. Significant improvements in friction behavior were obtained when properly biased films were deposited on deliberately preoxidized substrates. XPS depth profile data showed thick graded interfaces for bias deposited films even when adherence was poor. The addition of 10 percent hydrogen to the sputtering gas produced coatings with thin poorly adherent interfaces. Results suggest that some of the common practices in the field of sputtering may be detrimental to achieving maximum adherence and optimum composition for these refractory compounds.

Brainard, W. A.

On the sputtering of binary compounds

A simple physical model is presented to describe some aspects of the sputtering of compound targets. In particular, expressions are developed for the partial sputtering yields for binary systems in terms of the elemental sputtering rates, the stoichiometric concentrations, and surface binding energy. The partial yields depend nonlinearly on the bulk target concentrations. Comparison of the theoretical predictions with the data on sputtering of PtSi, NiSi, and Cu3Au indicates that the general features are well described.

Haff, P. K.

Ion beam sputter etching and deposition of fluoropolymers

Fluoropolymer etching and deposition techniques including thermal evaporation, RF sputtering, plasma polymerization, and ion beam sputtering are reviewed. Etching and deposition mechanism and material characteristics are discussed. Ion beam sputter etch rates for polytetrafluoroethylene (PTFE) were determined as a function of ion energy, current density and ion beam power density. Peel strengths were measured for epoxy bonds to various ion beam sputtered fluoropolymers. Coefficients of static and dynamic friction were measured for fluoropolymers deposited from ion bombarded PTFE.

Banks, B. A.