Reorientation of Randomly Oriented MoSx Coatings During Fretting Wear Tests

The reorientation of as-deposited randomly oriented sulphur-deficient MoS_x coatings during fretting wear tests has been investigated by X-ray diffraction (XRD), Scanning Electron Microscope and Transmission Electron Microscope. The driving force for the reorientation seems to be the plastic deformation induced by the tangential friction force during fretting tests. The evolution from an as-deposited randomly orientation into a basal one occurs above a threshold normal load and fretting frequency. This reorientation results in a lowering of the coefficient of friction as well as in a high resistance to humidity, but unfortunately a high wear rate is noticed. The effect of normal load and fretting frequency on that reorientation process in MoS_x coatings is discussed.     

Antiwear Properties of Bonded MoS2 Solid Lubricant Coating under Dual-Rotary Fretting Conditions

Bonded MoS₂ solid lubricant coatings are widely used in tribology for their friction-reducing and antiwear properties. However, such coatings have been rarely investigated in complex fretting conditions, such as dual-rotary fretting (DRF). DRF is a complex fretting wear mode that combines torsional fretting with rotational fretting. In this work, the antiwear properties of bonded MoS₂ solid lubricant coating under dual-rotary fretting conditions were studied. Results indicated that the MoS₂ coating had better friction-reducing and antiwear properties than the substrate for alleviating DRF wear. The coating can greatly influence the fretting regimes and reduce the coefficient of friction. Furthermore, the service life of the coating was strongly dependent on the competition of the two fretting components and was reduced as the rotational fretting component increased.     

Super-low friction of MoS2 coatings in various environments

The ultra-low friction coefficient (typically in the 10⁻² range) of MoS₂-based coatings is generally associated with the friction-induced orientation of ‘easy-shear’ planes of the lamellar structure parallel to the sliding direction, particularly in the absence of environmental reactive gases and with moderate normal loads. We used and AES/XPS ultra-high vacuum tribometer coupled to a preparation chamber, thus allowing the deposition of oxygen-free MoS₂ PVD coatings and the performance of friction tests in various controlled atmospheres. Friction of oxygen-free stoichiometric MoS₂ coatings deposited on AISI 52100 steel was studied in ultra-high vacuum (UHV: 5 × 10⁻⁸ Pa), high vacuum (HV: 10⁻³ Pa), dry nitrogen (10⁵ Pa) and ambient air (10⁵ Pa). ‘Super-low’ friction coefficients below 0.004 were recorded in UHV and dry nitrogen, corresponding to a calculated interfacial shear strength in the range of 1 MPa, about ten times lower than for standard coatings. Low friction coefficients of about 0.013–0.015 were recorded in HV, with interfacial shear strength in the range of 5 MPa. Friction in ambient air leads to higher friction coefficients in the range of 0.2. Surface analysis performed inside the wear scars by Auger electron spectroscopy shows no trace of contaminant, except after friction in ambient air where oxygen and carbon contaminants are observed. In the light of already published results, the ‘super-low’ friction behaviour (10⁻³ range) can be attributed to superlubricity, obtained for a particular combination of cystallographic orientation and the absence of contaminants, leading to a considerable decrease in the interfacial shear strength.     

Effect of deposition pressure on microstructure and tribological behavior of MoS<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>/MoS<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>-Mo nanoscale multi-layer films

MoS _x /MoS _x -Mo multi-layer films consisted of several bilayers and a surface layer on steel substrate were deposited by d.c. magnetron sputtering at different deposition pressures. Each bilayer contained a MoS _x layer with 80 nm in thickness and a MoS _x -Mo composite layer with 20 nm in thickness. With the increase of deposition pressure, the perpendicular orientation of the basal plane prevailed while the parallel orientation decreased. The tribological properties of the multi-layer films were investigated by using a ball-on-disk tribometer both in vacuum and in humid air. The multi-layer film deposited at 0.24 Pa had a compact, consistent layered structure with high intensity of (002) plane and low S content compared to the others deposited at 0.32 and 0.40 Pa, and showed the lowest friction coefficient and wear rate in humid air.     

In Situ Analysis of Third Body Contributions to Sliding Friction of a Pb–Mo–S Coating in Dry and Humid Air

Reciprocating sliding tests of ion-beam deposited (IBD) Pb–Mo–S coatings were performed with an in situ tribometer that allows real-time visualization and Raman analysis of the sliding contact through a transparent hemisphere. Experiments were performed in dry air, ambient air (∼50% RH) and mixtures of dry and humid air cycled between low and high humidity. Third bodies formed in the sliding contact were monitored through an optical microscope and analyzed by Raman Spectroscopy. Third body velocity accommodation modes were identified and correlated with friction behavior in dry and ambient air. The dominant velocity accommodation mode in both dry and humid air was interfacial sliding between the outer surface of the transfer film and the wear track; this interface, based on present and earlier studies, is crystalline MoS₂. Therefore, the friction coefficient was controlled by the interfacial shear strength of MoS₂ sliding against MoS₂. Humid air sliding was accompanied by a rise in the friction coefficient and a small but observable second velocity accommodation mode: shear/extrusion of the transfer film. It is concluded that the friction rise in humid air was due to an increase in the interfacial shear strength, and that the rise in friction caused the third body to deform rather than the deformation causing the friction to rise.     

Tribological Properties of Nanocomposite CrC<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>/a-C:H Thin Films

Recently we showed that coatings, prepared by unbalanced magnetron sputtering from a metallic Cr target in an Ar/CH₄ discharge are composed of nanocrystalline CrC _x embedded in an a-C:H matrix. This work investigates the structural correlation of such nanocomposite CrC _x /a-C:H coatings to their tribological properties. Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to characterize the phase composition and the chemical bonding in the films deposited at different experimental conditions. The coating microstructure was investigated on selected samples by high-resolution transmission electron microscopy. For CrC _x -dominated coatings deposited at CH₄ partial to total pressure ratios (p_CH4/p_t) < 0.42, only minor changes regarding the friction coefficients and the abrasive wear rates were observed although microstructural changes towards a higher degree of crystallinity were proven by transmission electron microscopy and substantiated with XPS results. For a-C:H dominated coatings deposited at p_CH4/p_t > 0.42, the friction coefficients and abrasive wear rates were shown to decrease with increasing a-C:H phase content and its more sp²-like bonding configuration. It can be concluded that the microstructural changes in terms of CrC _x crystallite coarsening and bonding configuration of the a-C:H matrix phase are responsible for the observed changes of the friction coefficients and wear rates.     

Tribological characterisation of hard coatings with and without DLC top layer in fretting tests

The potential of coatings to protect components against wear and to reduce friction has led to a large variety of protective coatings. In order to check the success of coating modifications and to find solutions for different purposes, initial tests with laboratory tribometers are usually done to give information about the performance of a coating. Different Ti‐based coatings (TiN, Ti(C,N), and TiAlN) and NiP were tested in comparison to coatings with an additional diamond‐like carbon (DLC) top coating. Tests were done in laboratory air at room temperature with oscillating sliding (gross slip fretting) with a ball‐on‐disc arrangement against a ceramic ball (Al₂O₃). Special attention was paid to possible effects of moisture (relative humidity). The coefficient of friction was measured on line, and the volumetric wear at the disc was determined after the test from microscopic measurements of the wear scar and additional profiles. The friction and wear behaviour is quite different for the different coatings and depends more or less on the relative humidity. The DLC coating on top of the other coatings reduces friction and wear considerably. In normal and in moist air the coefficient of wear of the DLC top‐layer coating is significantly less than 10⁻⁶ mm³/Nm and the coefficient of friction is below 0.1. In dry air, however, there is a certain tendency to high wear and high friction. Copyright © 2006 John Wiley & Sons, Ltd.     

Improving the Tribological Behavior of Graphite/Cu Matrix Self-Lubricating Composite Contact Strip by Electroplating Zn on Graphite

Studies to explore the nature of friction, and in particular thermally activated friction in macroscopic tribology, have lead to a series of experiments on thin coatings of molybdenum disulfide. Coatings of predominately molybdenum disulfide were selected for these experiments; five different coatings were used: MoS₂/Ni, MoS₂/Ti, MoS₂/Sb₂O₃, MoS₂/C/Sb₂O₃, and MoS₂/Au/Sb₂O₃. The temperatures were varied over a range from −80 °C to 180 °C. The friction coefficients tended to increase with decreasing temperature. Activation energies were estimated to be between 2 and 10 kJ/mol from data fitting with an Arrhenius function. Subsequent room temperature wear rate measurements of these films under dry nitrogen conditions at ambient temperature demonstrated that the steady-state wear behavior of these coatings varied dramatically over a range of K = 7 × 10⁻⁶ to 2 × 10⁻⁸ mm³/(Nm). It was further shown that an inverse relationship between wear rate and the sensitivity of friction coefficient with temperature exists. The highest wear-rate coatings showed nearly athermal friction behavior, while the most wear resistant coatings showed thermally activated behavior. Finally, it is hypothesized that thermally activated behavior in macroscopic tribology is reserved for systems with stable interfaces and ultra-low wear, and athermal behavior is characteristic to systems experiencing gross wear.     

Effect of current density,MoS2 content and bath agitation on tribological properties of electrodeposited nanostructured Ni-MoS2 composite coatings

ABSTRACT

Nanostructured nickel coatings with molybdenum disulphide particles were electrodeposited to form composite coatings. Three different current densities, i.e. 3, 5 and 7?A/dm² were investigated initially. The best results were obtained with 5 A/dm² for codeposition of nanostructured Ni-MoS₂ composite coatings. With the addition of 1–4?g/L molybdenum disulphide to the bath, the weight percentages of MoS₂ particles in the coatings were 23–38%. This increase of MoS₂ content was accompanied with decrease in friction coefficient of the coatings from 0.35 to 0.08. Wear resistance of the coatings was increased with increasing MoS₂ content and the weight loss was decreased from 1.4 to 0.7?mg. Hardness was decreased from 585 to 400 VHN with increasing the MoS₂ content. By increasing bath agitation speed up to 150?rpm, more MoS₂ particles were embedded in the matrix and the coatings showed better wear resistance. However, increase of agitation speed from 150 to 200?rpm caused a decrease of MoS₂ particles in the nickel matrix due to the turbulent motion of particles in the bath. Overall, it was shown that the lubricating effect of MoS₂ in the coating was more influential than the nanocrystallinity of the nickel matrix in improving tribological properties of these composite coatings.     

Experimental Evaluation of Friction and Wear Properties of Solid Lubricant Coatings on SUS440C Steel in Liquid Nitrogen

The friction and wear properties of the prevailing different solid lubricant coatings (Ion-plated Au, Ion-plated Ag and RF-sputtered PTFE on SUS440C stainless steel) used in the bearings of high-speed cryogenic-turbo-pumps of liquid rocket engines were experimentally evaluated in liquid nitrogen immersed conditions. Also the above experiments were carried out with two newly proposed solid lubricant coatings of sputter-ion-plated MoSTi and a new ion-plated Pb on SUS440C stainless steel. The friction coefficient and wear rates of the coatings of ion-plated Au, ion-plated Ag, RF-sputtered PTFE, the new ion-plated Pb and MoS₂Ti-SIP (with coating thickness of 0.7±0.1 μm) on SUS440C steel against SUS440C stainless steel ball in liquid nitrogen were compared. Worn surfaces were examined microscopically with a microscope and a profilometer for understanding the mechanisms of friction and wear and transfer film lubrication in liquid nitrogen. It is found that the newly proposed solid lubricant coatings are showing promising results for their use in liquid nitrogen immersed conditions. The sputter-ion-plated MoSTi coating on SUS 440C steel shows a minimum value of friction coefficient (μ=0.015) and wear rate (w_c=0.56 × 10⁻⁶ mm³/N m ) in liquid nitrogen.     

Study on rotational fretting wear of bonded MoS2 solid lubricant coating prepared on medium carbon steel

The rotational fretting wear behaviors of the bonded MoS₂ solid lubricant coating and its substrate steel were comparatively studied under varied angular displacement amplitudes, constant normal load, and rotational speed. Dynamic analysis in combination with microscopic examinations was performed through SEM, EDX, XPS, optical microscope, and surface profilometer. The experimental results showed MoS₂ changed the fretting running regimes of substrate. The friction coefficients of MoS₂ were lower than those of the substrate. For MoS₂, the damage in partial slip regime was very slight. The damage mechanism of the coating in slip regime was main abrasive wear, delamination, and tribo-oxidation.     

Torsional Fretting Wear Behavior of Bonded MoS2 Solid Lubricant Coatings

The effects of applying a bonded MoS₂ solid lubricant to a 1050 steel substrate were investigated using a torsional fretting wear apparatus. Tests were conducted under a normal load of 50 N with angular displacement amplitudes ranging from 0.1 to 5°. Wear scars were examined using scanning electron microscopy, energy-dispersive X-ray spectrometry, optical microscopy, and surface profilometry. The MoS₂ coating exhibited different torsional fretting regimes than those of the substrate. Fretting regimes of the coating were primarily in the partial slip regime (PSR) and the slip regime (SR) with no mixed fretting regime. The width of the PSR narrowed. Due to the lubricating effects of the coating, the friction torque was consistently lower than that of the substrate. The damage to the coating in the PSR was very slight, and its granular structure remained even after 1,000 cycles. The damage mechanism to the SR coating was a combination of abrasive wear, oxidative wear, and delamination. The MoS₂ coating had potential to alleviate torsional fretting wear.     

Tribological behaviour and wear mechanism of MoS2–Cr coatings sliding against various counterbody

MoS₂–Cr coatings with different Cr contents have been deposited on high speed steel substrates by closed field unbalanced magnetron (CFUBM) sputtering. The tribological properties of the coatings have been tested against different counterbodies under dry conditions using an oscillating friction and wear tester. The coating microstructures, mechanical properties and wear resistance vary according to the Cr metal-content. MoS₂ tribological properties are improved with a Cr metal dopant in the MoS₂ matrix. The optimum Cr content varies with different counterbodies. Showing especially good tribological properties were MoS₂–Cr8% coating sliding against either AISI 1045 steel or AA 6061 aluminum alloy, and MoS₂–Cr5% coating sliding against bronze. Enhanced tribological behavior included low wear depth on coating, low wear width on counterbody, low friction coefficients and long durability.     

DLC solid lubricant coatings on ball bearings for space applications

The environment of space offers special challenges for the lubrication of components in sliding and rolling mechanisms. Hydrogenated diamond-like carbon (DLC) films are being studied as solid lubricant coatings to simultaneously fulfil specifications regarding wear resistance and low friction behaviour under ambient atmosphere and in vacuum.In this paper, the tribological behaviour of highly hydrogenated DLC coatings (50 at% hydrogen) is assessed. Coating composition was optimised on flat AISI 52100 steel substrates based on ball-on-disc tribotest results in air, vacuum and dry nitrogen environments. The developed DLC coatings can be tailored to yield ultra-low friction values in vacuum (μ=0.008). The average friction coefficient range obtained in humid air, dry nitrogen and vacuum for the range of applied loads were, respectively, 0.22 to 0.27, 0.02 to 0.03, and 0.007 to 0.013.New in this work is that optimised DLC coatings were applied to ball bearings for space applications. The torque and life tests of coated pairs of angular contact bearings in air revealed that relatively high bearing torques are generated which increase with time, but the amount of coating wear generated during in-air operation appears relatively light. In vacuum, low torques are generated after a prolonged running-in period. Low-torque life exceeds that observed for MoS₂ by a factor of about two. It is concluded that, in contrast to MoS₂ coated bearings, DLC-coated bearings for space applications might therefore be capable of undergoing in-air ground testing without too much disruption of the subsequent in-space performance.     

Tribological characteristics of magnetron sputtered MoS2 films in various atmospheric conditions

The friction and wear behaviors of magnetron sputtered MoS₂ films were investigated through the use of a pin and disk type tester. The experiments were performed for two kinds of specimens (ground (Ra 0.5μm) and polished (Ra 0.01 μm) substrates) under the following operating condifions: linear sliding velocities in the range of 22 -66 mm/s(3 types), normal loads varying from 9.8-29.4 N(3 types) and atmospheric conditions of air, medium and high vacuum(3 types). Silicon nitride pin was used as the lower specimen and magnetron sputtered MoS₂ on bearing steel disk was used as the upper specimen. The results showed that low friction property of the MoS₂ films could be identified in high vacuum and the specific wear rate in air was much higher than that in medium and high vacuum due to severe oxidation. It was found that the main wear mechanism in air was oxidation whereas in high vacuum accumulation of plastic flow and adhesion, were the main causes of wear.     

The influence of humidity on the fretting behaviour of PVD TiN coatings

The influence of the relative humidity (RH) in ambient air on the friction and wear behaviour of PVD TiN coatings subjected to contact vibrations against corundum and bearing steel (100Cr6) counterbodies has been investigated. The fretting experiments were performed in the gross-slip regime on TiN coatings produced by three different PVD processes. The results indicate two basic friction characteristics. At low relative humidity (RH < 10%), the friction force is in the range of the normal force whereas it is less than one third of the normal force in atmospheres of high relative humidity (RH > 80%). A transition from high to low friction was observed during the course of experiments performed in atmospheres of medium relative humidity. The duration of the high friction phase in such transitions was found to depend on fretting parameters such as the normal force and the vibration frequency. This humidity dependence of the friction force was found for both counterbody materials. The size of the damaged surface area as well as the volumetric wear on the TiN coatings were found to be largest at low relative humidity. Fretting damage occurs over a smaller area but extends more into the depth at high relative humidity. The size of the fretted surface area induced on TiN is larger for Cr-steel than for corundum counterbodies.     

Environmental Effects on the Tribology and Microstructure of MoS<Subscript>2</Subscript>–Sb<Subscript>2</Subscript>O<Subscript>3</Subscript>–C Films

The tribology of molybdenum disulfide (MoS₂)–Sb₂O₃–C films was tested under a variety of environmental conditions (ambient 50% RH, 10⁻⁷ Torr vacuum, 150 Torr oxygen, and 8 Torr water) and correlated with the composition of the surface composition expressed while sliding. High friction and low friction modes of behavior were detected. The lowest coefficient of friction, 0.06, was achieved under vacuum, while sliding in 8 Torr water and ambient conditions both yielded the highest value of 0.15. Water vapor was determined to be the environmental species responsible for high friction performance. XPS evaluations revealed a preferential expression of MoS₂ at the surface of wear tracks produced under vacuum and an increase in Sb₂O₃ concentration in wear tracks produced in ambient air (50% RH). In addition, wear tracks produced by sliding in vacuum exhibited the lowest surface roughness as compared to those produced in other environments, consistent with the picture of low friction originating from well-ordered MoS₂ layers produced through sliding in vacuum.     

Effect of atmospheric pressure on friction and wear of 0.45% C steel in fretting

Oxidative wear is significant in fretting wear when sufficient oxygen is supplied. In vacuum, however, oxide does not form readily. In this paper friction and wear behaviours were studied at various atmospheric pressures in order to clarify the effect of ambient pressure on them.Experiments were conducted with 0.45% C steel at ambient pressures from 1.0 × 10⁵ to 1.3 × 10^?3 Pa. The load was 14 N, the peak-to-peak slip amplitudes were 35 and 110 μm and the frequency was usually 8.3 Hz.Friction behaviours are characterized into three types according to the ambient pressure: 1.0 × 10⁵ ? 10 Pa, 10 ? 10^?1 Pa and below 10^?1 Pa. The coefficient of friction increases with a decrease in ambient pressure below 1 Pa. The critical pressure in fretting is found to be 10 Pa, above which the oxidation rate is independent of the ambient pressure and α-Fe₂O₃ is formed. Wear decreases with ambient pressure below the critical pressure where Fe₃O₄ is formed. Adhesive transfer of metallic debris occurs below 10^?1 Pa.The relationship between the coefficient of friction and oxide thickness is obtained analytically, and the effect of frequency on the oxidation rate is considered.     

Friction, wear and N2-lubrication of carbon nitride coatings: a review

Recent results of tribological properties of carbon nitride (CN_x) coatings are reviewed. CN_x coatings of 100 nm thickness were formed on Si-wafer and Si₃N₄ disks by the ion beam mixing method. Friction and wear tests were carried out against Si₃N₄ balls in the environments of vacuum, Ar, N₂, CO₂, O₂ or air by a ball-on-disk tribo-tester in the load range of 80-750 mN and in the velocity range of 4-400 mm/s.It was found that friction coefficient μ is high (μ=0.2-0.4) in air and O₂, and low (μ=0.01-0.1) in N₂, CO₂ and vacuum. The lowest friction coefficient (μ<0.01) was obtained in N₂. It was also found that N₂ gas blown to the sliding surfaces in air effectively reduced the friction coefficient down to μ≈0.017. Wear rate of CN_x coatings varied in the range 10⁻⁹-10⁻⁵ mm³/N m depending on the environment.The wear mechanisms of CN_x in the nanometer scale were studied by abrasive sliding of an AFM diamond pin in air. It was confirmed that the major wear mechanism of CN_x in abrasive friction was low-cycle fatigue which generated thin flaky wear particles of nanometre size.     

A comparison of oxidation and oxygen substitution in MoS2 solid film lubricants

Significant advancements in the production of low friction, long wear life, sputter-deposited MoS₂ lubricant coatings have been made in the last decade. The introduction of multi-layered coatings, the establishment of careful controls on doping during DC and magnetron sputter deposition, and the implementation of ion assisted deposition have resulted in lubricants with substantially longer wear lives (up to a factor of ten greater than in the early 1980s) and lower sliding friction coefficients. A major research effort, designed to improve the performance of solid lubricants, involved a number of laboratories during this time period, resulting in these major breakthroughs. However, even with this concentrated effort, the typical investigation involved making an educated guess, based on previous experience, of the deposition conditions, target compositions, or post treatments that might be expected to provide improved performance of resulting coatings. One notable discovery during this time period was that typical MoS₂ films contain large quantities (up to 20 atom %) of oxygen substituted for sulfur in individual crystal lattices. In this paper we will compare the effects of this oxygen substitution with the effects of oxidation which involves a change in the oxidation number of the central molybdenum atoms within the crystals. A discussion of the relationship(s) between chemistry and coating structure and tribological performance will be presented with emphasis on defect chemistry and multiple phase interactions. Speculations on the role of coating chemistry in determining coating performance in applications such as in ball bearings will be presented.