Frictional and morphological properties of AuMoS2 films sputtered from a compact target

AuMoS₂ films 0.02–1.2 μm thick were sputtered from a target compacted from 5 wt.% Au plus 95 wt.% MoS₂ to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS₂ films are of interest to increase the densification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered AuMoS₂ and sputtered MoS₂ films have a tendency to break within the columnar region. The remaining or effective film, about 0.2 μm thick, performs the lubrication. The AuMoS₂ films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation compared with pure MoS₂ films. The more favorable frictional characteristics of the AuMoS₂ films are attributed to the effective film thickness and the high density packed columnar zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.     

Tribological characteristics of sputtered thin films in rolling hertzian contacts

The results of tribological studies carried out on hardened steel test bodies coated with solid lubricants are reported. The tests were carried out to assess the suitability of solid lubricant films in rolling hertzian contacts. A specially constructed concentrated contact simulator was used to determine the traction (frictional) characteristics of sputtered MoS₂ and WSe₂-In-Ga films. Test results obtained show that sputtered solid lubricant films are satisfactory for heavily loaded rolling contact applications as long as the slide-roll ratio is not very much larger than 0.02. Comparative tests show that burnished films yield lower traction coefficients than sputtered films indicating that there is room to improve sputtering practice further in order to enhance the tribological characteristics of sputtered solid lubricant films.     

Moisture-resistant MoS2-based composite lubricant films

The moisture resistance of sputter-coated composite films of MoS₂ can be markedly increased when the MoS₂ is sputter deposited with water-repellent additives. To increase the adhesion of such coatings and to prevent corrosive attack of the substrate, generally steel, a thin corrosion-resistant sulphide-forming intermediate layer is applied previously on the functional surface and serves as an interlayer.With a sputtering process coatings of these lubricants, which are durable in the Earth's atmosphere and adhere well to their support, are obtained. Friction and wear results for such composite lubricant films on different interlayers and various substrates, which were obtained in dry and humid air from pin and disc experiments and from functional bearing elements of precision engineering systems, confirm the improvements.     

Morphological and frictional behavior of sputtered MoS2 films

From the texture and growth patterns of sputtered MoS₂ films deposited onto substrates, three regions can be distinguised: (1) a ridge formation region, (2) an equiaxed transition zone and (3) a columnar-fiber-like structure. The lubricating properties of sputtered MoS₂ films can be visually identified with respect to optical changes before and after rubbing. The orientation of the surface microcrystallites is identified, and the change in optical properties is explained. In sliding contact the sputtered film tends to break up at the base of the columnar region. Effective lubrication occurs with the film remaining on the substrate. This film is 0.18–0.22 microm thick.     

Grundlageneigenschaften und Verschleißverhalten von HfB2- und Hf(B,N)-Schichtsystemen

Investigation of Fundamental Properties and Tribological Behaviour of HfB₂ and Hf(B,N) Coatings Thin films of HfB₂ and Hf(B,N), including intermediate layers of pure titanium, were sputtered in a rf sputtering unit on steel substrates. The deposition parameters bias-voltage and deposition pressure in the case of HfB₂ and the nitrogen flow concerning to Hf(B,N) were systematically varied. The characterization of the coatings includes fundamental properties such as thickness, hardness, adhesion and cohesion, structure, morphology, residual stresses and wear resistance of the coatings resulting from the plate on cylinder tribometer. The hardness values, analysed with the Vickers and the indentation depth method (Universal hardness), were extremely high for HfB₂ films, deposited with low deposition pressure or high bias voltage applied on the substrate. These results are probably caused by high residual stresses in the coating. The best wear properties could be obtained by testing the hardest coatings.     

H2S sensors based on SnO2 films: RGTO verses RF sputtering

Gas sensing characteristics of SnO₂ thin films prepared by RF sputtering have been investigated and compared to that of RGTO (Rheotaxially Grown and Thermally Oxidized) films. Both the sensor films exhibited a highly selective response towards H₂S with RF sputtered film showing better response characteristics. RF sputtered and RGTO films exhibited a maximum response of 54 and 15 towards 10 ppm of H₂S at an optimum operating temperature of 150 and 250 °C, respectively. Sputtered films exhibited a linear response in the wide concentration range from 500 ppb to 500 ppm while RGTO films were found to saturate for concentrations above 100 ppm. XPS investigations revealed that the RGTO films are more sub–stoichiometric or oxygen deficient than the sputtered films. Raman studies further indicates that the surface of sputtered and RGTO films are characterized by the presence of oxygen deficiency attributed to the “bridging-type” and deeper “in-plane/sub-bridging” oxygen vacancies, respectively. The improved response kinetics of the RF sputtered films is attributed to the presence of bridging type oxygen vacancies that facilitates the charge transfer between the sensor surface and H₂S molecules.     

Preparation of chameleon coatings for space and ambient environments

Tribological coatings of yttria-stabilized zirconia (YSZ), Au, diamond like carbon (DLC) and MoS₂ were synthesized using magnetron assisted pulsed laser deposition. The coatings were synthesized in four-component and three-component combinations that included YSZ/Au/DLC/MoS₂, YSZ/Au/MoS₂, and YSZ/Au/DLC. A range of coating compositions was studied to explore coating optimization for low friction in varying environments (dry, humid and high temperature). For four-component YSZ/Au/DLC/MoS₂ coatings, the optimal compositions for friction adaptation between dry nitrogen and humid air included relatively high concentrations of the soft phase, Au (> 20 at.%), and low amounts of the hard phases, DLC and YSZ. Ex situ Raman spectroscopy analysis indicates that friction adaptation involves a combination of both lubricating species, MoS₂ and carbon, where transitions of DLC to graphitic-carbon and amorphous MoS₂ to its hexagonal phase occur after cycling between both room temperature humid air and dry nitrogen. In large carbon concentrations (> 30 at.%), the DLC component was found to be detrimental for friction in dry nitrogen and humid air, but promoted a longer coating wear life at 500 °C. The three-component coating of YSZ/Au/MoS₂ performed well in both dry nitrogen and humid air, suggesting a synergism between Au and MoS₂, where carbon was not necessary for lubrication in humid air.     

Wear resistant composite coatings

In the search for wear resistant coatings, nanolaminated composite films composed of alternating metallic and ceramic layers, namely, Al/Al₂O₃ and Ti/TiN were produced using radio frequency magnetron sputtering. The metal layer thickness in the as-sputtered films of Al/Al₂O₃ ranged from 70 to 500 nm, and 150 to 450 nm in Ti/TiN. The non-metals (Al₂O₃ and TiN) layer thicknesses ranged from 10 to 40 nm and total film thicknesses of 10–15 µm. All coatings were characterized and tested for their tribological properties. Friction and wear tests were performed under non-lubricated sliding conditions using a pin-on-disc type tribometer. The coefficient of friction of the composite coatings tested, against a stainless steel pin, varied with the sliding distance. At the early stages of sliding the coefficient of friction rose to a peak, followed by a decrease to a steady-state value. Wear rates and coefficients of friction were related to the hardness and to the structure refinement of the coatings.     

Tribological behaviour of MoS2/Au coatings

This study aims to enhance the endurance of MoS₂ coating by applying a thin layer of Au (∼ 80 nm) on MoS₂ surface. Experimental results show that the addition of Au film increases the endurance of MoS₂/Au over equivalent coatings without Au. The friction coefficient rapidly decreases to a stable value (μ ∼ 0.045) after about 100 cycles sliding. After more than 15,000 cycles, the friction coefficient gradually increased to a second stable value (μ ∼ 0.15). An average endurance of over 50,000 cycles was measured in this case. The Au or Au-MoS₂ composite layer can effectively prevent oxygen or moisture reaction with MoS₂ and hence significantly increases the wear life.     

MoSx-Ta composite coatings on steel by d.c magnetron sputtering

Sputter-deposited MoS₂ films have been often used as dry lubricant in various industrial fields, such as space application and much attention has been paid to reduction of friction coefficient and improvement of mechanical properties in recent decades. One way to achieve this is to deposit a MoS₂ film doped with another metal. The MoS_x-metal films were found to be denser, more adhesive and more oxidation-resistant than pure MoS₂. In this study, MoS_x-Ta composite films were synthesized by Electron Cyclotron Resonance microwave source enhanced DC sputtering with different target powers. The effects of doping Ta on mechanical properties of MoS_x-Ta films were investigated. The morphology and structure of films were investigated using a scanning electron microscope (SEM), X-ray diffraction (XRD) and atomic force microscopy (AFM). The microhardness was evaluated using microhardness test instrument, and the adhesion strengths were obtained using a scratch tester. The results showed that the S/Mo ratio was influenced by the dc sputtering target power. Typical MoS₂ (100) (103) (002) orientations were present in pure MoS_x films, but disappeared with the increase in doped Ta, with the S/Mo content ratios decreasing from 1.52 to 0.84, and the hardness increasing from 3.55 to 15.23 GPa. The roughness and surface topography, friction coefficient and adhesion were significantly affected by the Ta, Mo and S content. The content of doped Ta plays a dominant role on the change in the Mo/S ratio, thereby influencing the mechanical and tribological properties of the MoS_x-Ta composite films.     

MoS2/ta‐C‐Kombinationsschichten hergestellt durch Laser‐Arc‐Technologie

MoS₂/ta‐C coatings produced by laserarc‐technology A series of MoS₂ and combined MoS₂/ta‐C coatings were prepared by lasercontrolled arc evaporation (Laser‐Arc) in order to study the tribological coating behaviour under vacuum and atmospheric conditions. Very low friction coefficients down to 0.005 were measured under high vacuum. By using a ta‐C underlayer beneath the MoS₂ a increased lifetime up to 5×10⁵ load cycles could be obtained. Also under atmospheric conditions the underlayer had a beneficial effect on coating performance.     

Highly adherent bioactive glass thin films synthetized by magnetron sputtering at low temperature

Thin (380–510 nm) films of a low silica content bioglass with MgO, B₂O₃, and CaF₂ as additives were deposited at low-temperature (150°C) by radio-frequency magnetron sputtering onto titanium substrates. The influence of sputtering conditions on morphology, structure, composition, bonding strength and in vitro bioactivity of sputtered bioglass films was investigated. Excellent pull-out adherence (~73 MPa) was obtained when using a 0.3 Pa argon sputtering pressure (BG-a). The adherence declined (~46 MPa) upon increasing the working pressure to 0.4 Pa (BG-b) or when using a reactive gas mixture (~50 MPa). The SBF tests clearly demonstrated strong biomineralization features for all bioglass sputtered films. The biomineralization rate increased from BG-a to BG-b, and yet more for BG-c. A well-crystallized calcium hydrogen phosphate-like phase was observed after 3 and 15 days of immersion in SBF in all bioglass layers, which transformed monotonously into hydroxyapatite under prolonged SBF immersion. Alkali and alkali-earth salts (NaCl, KCl and CaCO₃) were also found at the surface of samples soaked in SBF for 30 days. The study indicated that features such as composition, structure, adherence and bioactivity of bioglass films can be tailored simply by altering the magnetron sputtering working conditions, proving that this less explored technique is a promising alternative for preparing implant-type coatings.     

Thermal stability of sputtered Mo/polyimide films and formation of MoSe2 and MoS2 layers for application in flexible Cu(In,Ga)(Se,S)2 based solar cells

Molybdenum (Mo) films with a thickness of about 800 nm were room temperature sputtered onto flexible polymeric substrates. Upilex® films were chosen as substrates on the basis of their high thermal endurance and reduced coefficient of thermal expansion. Thermal stability of Mo films has been proved by heat treatment of the Mo/Upilex® structures at a temperature comparable to that used in the preparation of the Cu(In,Ga)(Se,S)₂ absorber layer. A combination of high optical reflectance (maximum values of 75-80%), low electrical resistivity (about 30 μΩ cm) and a smooth surface free of cracks for heated films highlights their good thermal stability. The formation of MoSe₂ and MoS₂ layers, after selenization/sulfurization of the Mo/Upilex® structures, has been further investigated in view of their application as back contact layers in flexible CIGS based solar cells.     

Transfer of molybdenum sulphide coating material onto corundum balls in fretting wear tests

Transfer films on corundum balls from sulfur deficient molybdenum disulfide (MoS_x) coatings with different crystallographic orientations were investigated after fretting tests performed in ambient air of different humidity levels. The morphology of wear tracks on MoS_x coatings and of transfer films on corundum balls were investigated by light optical microscopy with Normarski contrast. The thickness of transfer films was measured by scanning white light and optical phase-shifting interferometry, and their composition was analyzed by X-ray photoelectron spectroscopy. The effect of relative humidity in fretting tests on the composition of the transfer films as well as the effect of the transfer film on the tribological performance of MoS_x coatings in fretting wear tests is discussed.     

Superlubricity between MoS2 Monolayers

The ultralow friction between atomic layers of hexagonal MoS₂, an important solid lubricant and additive of lubricating oil, is thought to be responsible for its excellent lubricating performances. However, the quantitative frictional properties between MoS₂ atomic layers have not been directly tested in experiments due to the lack of conventional tools to characterize the frictional properties between 2D atomic layers. Herein, a versatile method for studying the frictional properties between atomic‐layered materials is developed by combining the in situ scanning electron microscope technique with a Si nanowire force sensor, and the friction tests on the sliding between atomic‐layered materials down to monolayers are reported. The friction tests on the sliding between incommensurate MoS₂ monolayers give a friction coefficient of ≈10^?4 in the regime of superlubricity. The results provide the first direct experimental evidence for superlubricity between MoS₂ atomic layers and open a new route to investigate frictional properties of broad 2D materials.     

Lubrication mechanisms of C‐MoS2‐Fe2O3 (Fe3O4) nano‐composite lubricants at the rubbing interfaces of non‐copper coated solid wires against the contact tube

Graphite‐MoS₂‐Fe₂O₃ (Fe₃O₄) nano‐composite lubricating coatings were prepared on the surfaces of non‐copper coated solid wires by a mechanical coating technique. The tribological behaviours of graphite‐MoS₂‐Fe₂O₃ (Fe₃O₄) coatings at the rubbing interfaces of welding wires against the contact tube were investigated. The results demonstrate that the lubricating properties of graphite‐Fe₃O₄ coatings outperform the lubricating properties of graphite‐Fe₂O₃ coatings. The anti‐wear performance of the contact tube is strengthened with increasing nano‐MoS₂ contents. Layers of protective tribofilms are formed at the rubbing interfaces of welding wires against a contact tube by tribochemical reaction among lubricants. The tribofilms are composed of FeO, MoO₃ and FeMoO₄ with excellent lubricating properties. They can avoid direct contact of welding wires against the contact tube, thus decreasing contact tube wear. With the transition of the contact tube wear from mild to severe, the dominant wear mechanisms of contact tube change from fatigue peeling and oxidative wear to abrasive wear and arc ablation.     

Effects of deposition parameters on hardness and lubrication properties of thin MoS2 films

The purpose of the present study is the development of a sputtered MoS₂‐coating suitable for the use in humid atmospheres. Influences of the process parameters argon pressure, temperature, distance between substrate and target and bias voltage on tribological properties and hardness are presented. By means of these parameter studies, different microstructures with widely varying wear behavior were achieved. Life cycle tests show that exclusively basal oriented coatings with dense, non columnar structures show the highest durability and a hardness of about 400 HV 0.01. However, dendritic needle like structures show lower endurance and lower hardness (<100 HV 0.01). Films with a comparatively high hardness (up to 800 HV 0.01) exhibit lowest sliding distances until failure due to an appearance of spalling in the ball‐on‐disc tests. Those coatings also show a dense but amorphous structure and sulfur deficiencies. Consolidation during sputtering, i. e. film hardness and porosity, can be controlled by certain process parameters and is probably affected by varying amounts of internal stress.     

Comparison of chromium nitride coatings deposited by DC and RF magnetron sputtering

Chromium nitride coatings were deposited by DC and RF reactive magnetron sputtering on AISI 304 stainless steels without substrate heating. A Cr₂N phase was formed in the RF sputtered coatings with a low N₂ flow content ranging within 30-50%. A NaCl type CrN_x phase was obtained by DC magnetron sputtering with different N₂ flow contents. The coating hardness increased with the increase of the N₂ flow content. When the coatings deposited with the same N₂ flow content were compared, the hardness of the RF sputtered CrN_x was higher than that of the DC sputtered CrN_x, which was mainly due to the distinct difference between the dense structure (RF process) and the porous structure (DC process). The RF sputtered CrN_x coatings showed an excellent adhesion strength as compared to the DC sputtered coatings. By selecting the deposition method and optimizing the N₂ flow content, CrN_x coatings with a preferred microstructure could be obtained, which would be a candidate material for research and applications in nano-science.     

PECVDTM Coatings in Industrial Applications

The adoption of GPI's Linear PECVD^TM process has accelerated over the last year. Several R&D and production reactor modules were installed at major companies and a turnkey in‐line system was completed. Through these installations, customers are confirming the superior deposition rate, uniformity and stability of Linear PECVD^TM compared to reactive sputtering. Today Linear PECVD^TM is being used to deposit oxide and nitride films on a variety of substrates. The films include SiO₂, TiO₂, Al2₂O₃, SiN, ZnO, and SnO and the applications include multi‐layer AR coatings, single layer oxides and nitrides in combination with sputtered films, thin‐film solar coatings, barrier films, anti‐smudge coatings and TCO's. This progress demonstrates that GPI's Linear PECVD^TM technology may soon displace reactive sputtering of oxides and nitrides for large area substrates in architectural glass, flat panel display and flexible web applications.     

Investigating the wear characteristics of engineered surfaces: low-temperature plasma nitriding and TiN + MoS x hard-solid lubricant coating

Significant progress has been made in the past decade in plasma nitriding with a majority of the research work focusing on improving hardness and wear resistance of the nitrided surface through the reduction of nitriding temperature, pressure or time. Hard-solid lubricating coatings have also been extensively studied for lowering the wear rate and coefficient of friction of traditional hard coatings such as TiN by the combined effect of hardness and solid lubrication. In this study, the wear characteristics of low-temperature plasma-nitrided steel substrate performed using a Saddle-field fast atom beam source and TiN + MoS _x hard-solid lubricant coating deposited by a closed-field magnetron-sputtering technique have been investigated. The thin hard layer in plasma-nitrided substrates exhibited much higher hardness and lower wear compared to the untreated substrate in pin-on-disc wear testing. In addition, the study of the wear track morphology of the nitrided samples evidenced significant reduction of deeper ploughing and plastic deformation due to higher hardness and load supporting of the nitrided layer. On the other hand, due to the incorporation of MoS₂ in TiN coating, the wear resistance and coefficient of friction were greatly improved in TiN + MoS _x coating compared to pure TiN coating. In contrast to TiN coating, a relatively smoother wear track with less abrasive wear also supported the beneficial effects of adding MoS₂ in TiN coating.