Adhesion and friction properties of hydrogenated amorphous carbon films measured by atomic force microscopy

Atomic force microscopy has been used to measure adhesion and friction forces at the interface between an oxidized metal probe tip and amorphous carbon films of varying hydrogen contents (12.3–39.0 atomic percent hydrogen). The interface of an oxide surface and a hard carbon coating models the unlubricated head-disk interface of current hard disk products. Adhesion forces normalized by the radius of curvature of the contacting tip range from 1.09 to 8.53 N/m. Coefficients of friction values, measured as the slope of the friction versus load plot, range from 0.33 to 0.87. A trend of increasing adhesion forces and coefficients of friction is observed for increasing hydrogen content in the films. We attribute the increase in adhesion and friction to increases in the surface free energy of the carbon films with the incorporation of hydrogen.     

Mechanical and tribological properties of amorphous carbon films

The mechanical and tribological properties of amorphous carbon films have been studied in more detail in recent years because these films (a) can be deposited near room temperature, thus allowing film deposition on common engineering alloys (i.e., aluminum and steel) without altering their mechanical properties, and (b) are smooth and conform to surface roughness of the substrate, thus requiring no post deposition processing. In addition, amorphous carbon films exhibit low unlubricated sliding friction in contact with steel and ceramics which is comparable to that of steel against steel in a lubricated contact. The wear resistance of these films is also better than Ti‐based hard coatings. Further improvement in film tribological properties can be achieved by modifying film chemical composition. Because of these attractive features, amorphous carbon films have been evaluated in several applications including automotive, electronic and biomedical engineering. However, environmental factors such as oxygen and humidity have been found to influence tribological properties significantly. This paper reviews the current understanding of the tribological properties of both hydrogenated and non‐hydrogenated amorphous carbon films, the mechanisms responsible for low friction coefficient and identifies areas that require further research. This revised version was published online in June 2006 with corrections to the Cover Date.     

Nano-wear mechanism of amorphous carbon thin films

Tribological performance of diamond-like carbon (DLC) overcoat on a magnetic hard disk was evaluated using a contact start stop wear tester. The analysis of worn surfaces suggests that wear of the carbon overcoat took place by a delamination type of wear mechanism at a nanoscale, resulting in the formation of wear particles of about 1.5 nm thick and 30–90 nm wide. This revised version was published online in July 2006 with corrections to the Cover Date.     

Nano-scratching process and fracture mechanism of amorphous carbon films

The nano-scratch behavior of amorphous carbon films prepared on Ti alloy substrate by rf PECVD was evaluated using a nano indenter system with an attachment for lateral force measurement. The scratching processes were analyzed to understand the deformation behavior and the failure mechanism of the films. It was concluded that, three processes containing fully elastic recovery, asynchronous recovery, and delaminating of the film, successively occurred with the increase of load during scratching; in the first regime, no damage could be found on the surface of the film, in the second regime, due to asynchronous recovery of the film and the substrate, a trace like fish bone was formed, which was composed of tiny cracks along the track of the indenter. It was only in the third regime that the critical load was reached and partial spalliation of the film was detected with careful examination. It was determined that the film spalliation originated right from the fish bone cracking, and the fish bone was just a profiling of the Berkovich indenter. By our model, the film was delaminated from the substrate due to combining effect of parallel cracks and the separation of the interface between the film and the substrate.     

Comparative studies of perfluorinated lubricants adsorbed on hydrogenated amorphous carbon and amorphous carbon nitride

Temperature-programmed desorption and scanning force microscopy have been used to probe the interaction of a perfluorinated lubricant (Fomblin ZDOL) with hydrogenated amorphous carbon (a:C-H _x ) and amorphous carbon nitride (a:C-N _x ) substrates, two materials used as hard coatings in disk drive products. Temperature-programmed desorption measurements indicate that the nitride surfaces are more reactive toward this perfluorinated lubricant and, as a result, the thin lubricant film is more tightly bound to this substrate. Frictional force microscopy has been used to measure the coefficient of friction of the lubricated surfaces, 0.18 ± 0.02 for both substrate materials, and finds that frictional properties of these interfaces in the low load regime are influenced more by the presence of the lubricant rather than the adsorbed state of the film. Likewise, similar disjoining pressures were measured for the lubricant adsorbed on the different coating materials and suggest that the ultrathin nature of the adsorbed lubricant film dominates this property rather than adsorption states.     

Measurements of tribological properties of poly(pyrrole) thin film bearings

We report the results of a recent study on the tribological properties of electropolymerised thin films at light loads and low speeds. Poly(pyrrole) films incorporating different counter-ions have been electrochemically deposited onto gold electrodes on the plano-convex glass substrates and studied extensively. The measuring apparatus has been greatly improved from that reported earlier and now provides simultaneous monitoring of frictional force and wear. High precision capacitive gauging is employed to provide high resolutions of frictional force of better than 100 μN and height variation (wear) of 2 nm. A large number of specimens of poly(pyrrole) grown from five different counter-ions were prepared and their performances evaluated. The film morphology of each type of film was examined by atomic force microscopy (AFM) for control of the variability of film formation. Results are presented for the friction coefficients and wear rates observed for the films typically at a load of 2 N and a sliding speed of 5 mm s⁻¹. The effects of normal loading force and sliding speed on the friction coefficient are also discussed with a load range of 0.2–5 N and a sliding speed up to 30 mm s⁻¹.     

Effects of surface forces on pure squeeze thin film EHL motion of circular contacts

The pure squeeze thin film elastohydrodynamic lubrication (thin film EHL) motion of circular contacts with effects of surface forces taken into account is explored under constant load conditions. The difference between thin film EHL model and EHL model is apparent as the film thickness is thinner than 5 nm. The oscillation phenomena in pressure and film thickness come mainly from the action of solvation forces. The effects of surface forces become significant as the film thickness becomes thinner. Moreover, the viscosity is oscillatory due to its dependency on the hydrodynamic pressure which is affected by surface forces.     

Optimum film thickness of thin metallic coatings on silicon substrates for low load sliding applications

The frictional behaviour of thin metallic films on silicon substrates sliding against 52100 steel balls is presented. The motivation of this work is to identify an optimum film thickness that will result in low friction under relatively low loads for various metallic films. Dry sliding friction experiments on silicon substrates with soft metallic coatings (silver, copper, tin and zinc) of various thickness (1–2000 nm) were conducted using a reciprocating pin-on-flat type apparatus under a controlled environment. A thermal vapour deposition technique was used to produce pure and smooth coatings. The morphology of the films was examined using an atomic force microscope, a non-contact optical profilometer and a scanning electron microscope. Following the sliding tests, the sliding tracks were examined by various surface characterization techniques and tools. The results indicate that the frictional characteristics of silicon are improved by coating the surface with a thin metallic film, and furthermore, an optimum film thickness can be identified for silver, copper and zinc coatings. In most cases ploughing marks could be found on the film which suggests that plastic deformation of the film is the dominant mode by which frictional energy dissipation occurred. Based on this observation, the frictional behaviour of thin metallic coatings under low loads is discussed and friction coefficients are correlated with an energy based friction model.     

Amorphous hydrogenated carbon films for tribological applications I. Development of moisture insensitive films having reduced compressive stress

Although earlier investigations on the tribological behaviour of amcrphous hydrogenated carbon (AHC) films in sliding contact with steel showed encouraging results, four open issues were identified. They were: (a) dependence of friction and wear on humidity (i.e., the friction coefficient and the wear increased with humidity), (b) limitations on film thickness (i.e., films greater than 2 μm thick delaminated due to large compressive stress), (c) deposition of films on substrates other than silicon and (d) lubricant compatibility (i.e., formation of lubricant-derived antiwear films on AHC film surfaces). Steps were taken to address some of these open issues by incorporating silicon in AHC films. Friction and wear tests were conducted on AHC films containing various amounts of silicon. Incorporation of silicon in AHC films rendered the friction coefficients and the wear of a steel counterface insensitive to moisture. Silicon incorporation in AHC films also significantly reduced compressive stress. This allowed deposition of 10 μm thick films. These effects were achieved without any compromise with the friction coefficient and the film wear if the amount of silicon in the film was kept within a certain concentration range. In addition, silicon-containing AHC films were thermally more stable than silicon-free films. Experiments conducted with two lubricants resulted in significantly lower wear of the silicon-free AHC films than that obtained for unlubricated sliding. Similar friction coefficients were obtained for AHC film/steel and steel/steel combinations in lubricated sliding.     

Genesis of superlow friction and wear in diamondlike carbon films

Diamondlike carbon (DLC) films offer enormous possibilities for applications that require low friction and high wear resistance. The range of physical, chemical, mechanical, electrical, and optical properties offered by these films is also exceptional and can meet the increasingly multifunctional application needs of machine elements, microelectronics, and biological systems. Since the early 1990s, carbon has been used as a precursor in our laboratory for the design and synthesis of superhard and low-friction carbon films. As a result of systematic studies over the years, in 1997, we developed a new class of DLC films that provide friction and wear coefficients of 0.001–0.005 and 10⁻¹⁰–10⁻⁹ mm³/N m, respectively, in inert-gas or vacuum test environments. This paper will mainly concentrate on the tribology of these superlow-friction carbon films and provide an update on our understanding of the fundamental tribological mechanisms of such films. It will also expand on the effects of hydrogen within the films and gaseous species within the test environments on friction and wear.     

A scanning conduction microscopic method for probing abrasion of insulating thin films

The use of scanning force microscopy (SFM) to probe wear processes at interfaces is of considerable interest. We present here a simple modification of the SFM which allows us to make highly spatially resolved measurements of conductivity changes produced by abrasion of thin insulating films on metal substrates. The technique is demonstrated on fluorocarbon polymer thin films deposited on stainless steel substrates.     

Mechanical properties of amorphous carbon nitride thin films prepared by reactive magnetron sputter-deposition

Nanoindentation hardness and compressive stress in amorphous carbon nitride thin films prepared by unbalanced magnetron sputter-deposition were studied. The coating hardness and compressive stress were found to be strongly dependent on processing parameters such as substrate bias and nitrogen partial pressure. Under optimized deposition conditions, carbon nitride thin films with nanoindentation hardness about 25 GPa have been coated onto Si wafers and M2 steels. A strong correlation between coating hardness and compressive stress in the coating was observed.     

Small amplitude reciprocating wear performance of diamond-like carbon films: dependence of film composition and counterface material

Small amplitude (50 μm) reciprocating wear of hydrogen-containing diamond-like carbon (DLC) films of different compositions has been examined against silicon nitride and polymethyl-methacrylate (PMMA) counter-surfaces, and compared with the performance of an uncoated steel substrate. Three films were studied: a DLC film of conventional composition, a fluorine-containing DLC film (F-DLC), and silicon-containing DLC film. The films were deposited on steel substrates from plasmas of organic precursor gases using the Plasma Immersion Ion Implantation and Deposition (PIIID) process, which allows for the non-line-of-sight deposition of films with tailored compositions. The amplitude of the resistive frictional force during the reciprocating wear experiments was monitored in situ, and the magnitude of film damage due to wear was evaluated using optical microscopy, optical profilometry, and atomic force microscopy. Wear debris was analyzed using scanning electron microscopy and energy dispersive spectroscopy. In terms of friction, the DLC and silicon-containing DLC films performed exceptionally well, showing friction coefficients less than 0.1 for both PMMA and silicon nitride counter-surfaces. DLC and silicon-containing DLC films also showed significant reductions in transfer of PMMA compared with the uncoated steel. The softer F-DLC film performed similarly well against PMMA, but against silicon nitride, friction displayed nearly periodic variations indicative of cyclic adhesion and release of worn film material during the wear process. The results demonstrate that the PIIID films achieve the well-known advantageous performance of other DLC films, and furthermore that the film performance can be significantly affected by the addition of dopants. In addition to the well-established reduction of friction and wear that DLC films generally provide, we show here that another property, low adhesiveness with PMMA, is another significant benefit in the use of DLC films.     

Topography and nanomechanical properties of tribochemical films derived from zinc dialkyl and diaryl dithiophosphates

In this paper we present recent results from an on‐going effort to characterize the nanomechanical properties of a variety of tribochemical, antiwear films through the use of modern scanning probe techniques. The two types of antiwear wear films studied, derived from zinc dialkyl dithiophosphate (alkyl ZDDP) and zinc diaryl dithiophosphate (aryl ZDDP), were chosen because they possess significantly different wear characteristics. High resolution AFM topographic images showed significant differences between the two types of films. More interestingly, high resolution imaging and quantitative mechanical properties testing using the interfacial force microscope (IFM), revealed different elastic and plastic properties between the two types of films; in addition each type of film possessed several distinct regions with respect to mechanical properties. The maximum values for elastic modulus and hardness were located on the highly loaded regions of the alkyl ZDDP films which exhibited the best tribological performance. In contrast, the aryl ZDDP films, which exhibited poorer antiwear behaviour, were devoid of such resilient regions. Our results correlate the macroscopic wear behavior of the tribochemical films to differences in the mechanical properties on a nanometer scale. This revised version was published online in July 2006 with corrections to the Cover Date.     

Amorphous hydrogenated carbon films for tribological applications II. Films deposited on aluminium alloys and steel

This paper describes the methods for the deposition of AHC films on aluminium alloys (2024, 7075 and an additional Al-Si alloy) and AISI 4340 steel. Both unmodified and silicon modified AHC films were deposited. AHC films could be deposited on aluminium alloys without any interlayer. The deposition of AHC films on steel required an interlayer which could be aluminium, silicon or chromium. Thin films (1–2 μm) deposited on aluminium alloys and steel influenced durability of films and friction coefficients in contact with steel. These were believed to be due to plastic deformation of substrates. Deposition of a thicker coating system (interlayer + AHC) reduced friction coefficients and also improved film durability. The durability of films deposited on steel substrates was evaluated under both unlubricated and lubricated conditions for 5.5 million cycles under 4.4 N load and up to 2.5 m/s sliding speed. Although there was wear, the films survived 5.5 million test cycles under unlubricated sliding, but in the presence of two lubricants, the film wear was very small and could not be measured. It was observed that the wear of the steel counterface in contact with silicon-containing AHC films could be higher than that against an uncoated steel in the presence of certain lubricants.     

The influence of thin boundary films on real surface roughness in thin film, mixed EHD contact

The behaviour of thin viscous boundary films in the rough surface rolling–sliding point contact operated under thin film lubrication conditions have been observed by thin film colorimetric interferometry. Changes in film thickness distribution within the lubricated contact between steel ball and glass disc were studies with both mineral base oil and mineral oil formulated with non-functionalized polyalkylmethacrylate (PAMA). Recent studies by other researchers showed that this polymer-containing viscosity index improver exhibits some friction-reducing capabilities even though it forms only very thin boundary films on rubbing surfaces. Results obtained in the current study proved that thin viscous boundary films formed on rubbing surfaces can reduce asperities interactions of rubbing surfaces under very thin film conditions. Even though these boundary films do not separate rubbing surfaces completely, they still can provide some protection of contacting bodies against excessive friction and wear.     

Precise and reproducible deposition of thin and ultrathin carbon films by flash evaporation of carbon yarn in high vacuum

A simple, small device and its use for reproducible flash evaporation of carbon yarn in high vacuum are characterized. Using this flash evaporator, carbon films of any thickness up to 20 nm can be deposited without spark generation under minimized photon radiation, and with an accuracy better than ±0·2 nm. The films have less background structure (imaged in phase contrast) than conventionally rod evaporated films and are therefore suitable for many kinds of thin and ultrathin carbon film applications in electron microscopy, e.g. as backing for formvar films or sections, as isolating carbon layers for autoradiography, as ultrathin films (floated from mica) for support of macromolecules to be metal shadowed and as support and cover for negative staining of various specimens by the sandwich technique.     

Tribochemical effects on the friction and wear behaviors of a-C:H and a-C films in different environment

Friction and wear behaviors of hydrogenated amorphous carbon (a-C:H) and hydrogen-free amorphous carbon (a-C) films sliding against Si₃N₄ balls were investigated in different testing environments. The result showed that two films with extreme chemical disparity (one hydrogenated, and the other hydrogen free) showed distinct different friction and wear behaviors, and the friction and wear behaviors of the both films were strongly dependent on the environment. For a-C:H films, much low friction coefficient and wear rate were obtain in dry N₂. In the water and/or oxygen containing environments, the friction coefficient and wear rate of a-C:H films were obviously increased. On the contrary, a-C films only provided low friction coefficient and wear rate in the presence of water and/or oxygen in the test chamber. In dry N₂, the highest friction coefficient and wear rate were observed for a-C films. By investigating the worn surfaces of the films using XPS, it was proposed that the environment dependence of the friction and wear behaviors of the films was closely related with the friction-induced chemical interactions between the films and water and/or oxygen molecules. The specific roles of hydrogen, water and oxygen molecules and their tribochemical effects on the friction and wear mechanism of the films are discussed.     

Micro- and macro-tribological properties of SiC ceramics in sliding contact

Surface properties of single-crystalline and polycrystalline silicon carbide (SiC) specimens were measured using atomic force/friction force microscopy, Auger electron spectroscopy and nano-indentation techniques. Running-in behavior during sliding tests in vacuum was studied on self-mated SiC pairs as a function of surface quality produced by machining. Tribological mechanisms were analyzed in short-time tests using a high-resolution micro-tribometer and then were related to results obtained from macro-tribological tests in humid air and in the presence of distilled water. Information on the structure, chemical composition and properties of SiC surfaces resulting from measurements on the nanoscale can be very useful for explaining tribological performance under far different operating conditions such as in vacuum or air, with contact areas ranging from diameters of a few nanometers to one millimeter and initial applied contact pressure from about 1 MPa to 3 GPa. Friction and wear mechanisms are discussed as functions of surface composition and roughness, vacuum and humidity of air.     

Effects of humidity on nano-oxidation of silicon nitride thin film

Effects of humidity on nanometer-scale oxidation of silicon nitride thin film using atomic force microscope in contact mode are studied at various values of relative humidity (RH) (30-70%). The shape of oxide protrusion is determined by the concentration of oxyanions under the tip apex and oxyanions diffusion laterally on the surface. At low RH (60%), the kinetics of silicon nitride oxidation has a logarithmic relationship to oxide height versus oxidation time. The threshold time decreased and initial oxidation rate increased simultaneously as humidity increased because a high concentration of oxyanions at the oxide/silicon nitride interface was generated. When a high sample voltage (9-10V) is applied at high RH (60%), the effective electric field is decreased because of the electron being trapped in the oxide and oxyanions accumulating on the oxide surface.