Stresses in diamond-like carbon films

Internal stresses have been measured in diamond-like carbon (DLC) films deposited by d.c. plasma assisted chemical vapor deposition from methane, acetylene, or cyclohexane, and in nitrogen containing DLC films deposited from acetylene, or cyclohexane and nitrogen. The total hydrogen content in the films and the fraction of bound hydrogen have been analyzed by forward recoil elastic scattering and Fourier transform infrared spectroscopy respectively. It was found that in pure DLC films the stresses increase with increasing fraction of unbound hydrogen. The highest compressive stresses were obtained in the films deposited from methane and the lowest stresses in films deposited from cyclohexane. In the nitrogen containing DLC films the stresses decrease with increasing nitrogen content in the films. Stresses as low as 0.22 GPa were obtained in the films deposited from cyclohexane and nitrogen at a ratio of 1/15 in the plasma.     

Nano-texture for a wear-resistant and near-frictionless diamond-like carbon

The effect of nano-scale surface texture on wear resistance of diamond-like carbon (DLC) films was studied using a reciprocating ball-on-flat tribometer in dry, humid, and liquid water environments. The nano-scale surface texture was produced by depositing ∼1 μm thick DLC films onto silicon substrates pre-textured with pyramidal wells and polystyrene spheres. The surface roughness of the textured DLC films was about 50 nm in both cases. The friction and wear behavior of the flat and nano-textured DLC films were tested with AISI 440C-grade stainless steel balls at a contact load creating about 360 nm deep Hertzian deformation which is significantly larger than the surface roughness. At this condition, nano-texturing did not affect the friction coefficient, but it significantly reduced the wear of DLC films in dry and humid nitrogen compared to flat DLC. In dry nitrogen, the nano-textured DLC films showed the ultra-low friction without substantial wear of DLC and deposition of thick transfer films onto the counter-surface. The wear reduction appeared to be related to the stress relief in the nano-textured DLC film. In liquid water, surface features on the nano-textured DLC films were diminished due to tribochemical oxidation and material removal at the sliding interface.     

Nanotribological study of PECVD DLC and reactively sputtered Ti containing carbon films

Amorphous carbon film, also known as DLC film, is a promising material for tribological application. It is noted that properties relevant to tribological application change significantly depending on the method of preparation of these films. These properties are also altered by the compositions of these films. DLC films are well known for their self-lubricating properties, as well. In view of this, the objective of the present work is to compare the tribological properties of diamond like carbon (DLC) film obtained by plasma enhanced chemical vapour deposition (PECVD) with the Ti containing nanocrystalline carbon (Ti/a-C:H) film obtained by unbalanced magnetron sputter deposition (UMSD) in nN load range. Towards that purpose, DLC and Ti/a-C:H films are deposited on silicon substrate by PECVD and UMSD processes respectively. The microstructural features and the mechanical properties of these films are determined by scanning electron microscope (SEM), transmission electron microscope (TEM) and nano indenter. The surface topographies and the friction force surfaces of these films are evaluated by means of an atomic force microscope (AFM). The results show that although PECVD DLC film has higher elastic modulus and higher hardness than UMSD Ti/a-C:H film, the surface roughness and the friction coefficient of PECVD film is significantly higher than that of UMSD Ti/a-C:H film.     

Synthesis of amorphous carbon films by plasma-based ion implantation with simultaneous application of DC and pulse bias

Carbon films were synthesized on a Si wafer by simultaneous application of pulse bias and DC bias by a plasma-based ion implantation system using an electron cyclotron resonance (ECR) plasma source with a mirror field. The relationship between the pulse biasing voltage and the properties of carbon films was investigated. The hardness and tribological properties of the carbon film improved as the pulse bias voltage was decreased from −10 kV to −2 kV. Diamond-like carbon (DLC) films with a low friction coefficient were formed by simultaneous application of a low pulse bias voltage, such as −2 kV, and a DC bias. During the friction test of the DLC film, excellent tribological properties were observed under a high conducted load, such as 20 N, which shows that not only the friction coefficient but also the durability during the friction test was improved. The improvement of the tribological property was attributed to the formation of a mixed layer at the interface between the DLC film and the Si substrate.     

The effect of annealing on mechanical and tribological properties of diamond-like carbon multilayer films

The diamond-like carbon (DLC) multilayer films have been deposited by plasma CVD deposition onSi wafer substrate. The deposited films have then been post-annealed in vacuum at 250 °C for 2 h. Changes in internal stress, hardness, critical load, friction coefficient and wear have been investigated toassess the influence of annealing on mechanical and tribological properties of DLC multilayer films. At the same time, DLC single layerfilms are also deposited and annealed in the same method for a comparison.The results show that there is 28–33% decrease in internal stress and 10–13% decrease in hardness of theDLC single layer films after the anneal treatment. However, for the DLC multilayer films, there is 41–43% decreasein internal stress and less than 2% decrease in hardness. In addition, the annealed DLC multilayer filmhas the same friction and wear properties as that un-annealed film. This result indicates that the anneal treatment isan effective method for the DLC multilayer films to reduce the internal stress and to increase the critical load.The by-effect of the annealing, decrease of hardness and wear resistance of the multilayer film, can be restrictedby the multilayer structure.     

Superlow friction and diffusion behaviors of a steel-related system in the presence of nano lubricant additive in PFPE oil

The lubrication performances of diamond like carbon (DLC) films were investigated by a ball-on-disc tribometer under perfluoropolyether (PFPE) oil lubrications. The influence of nano lubricant additives in PFPE oil on the tribological properties of DLC films was evaluated. The experimental results show that the solid-liquid synergy lubrication is beneficial to improve the tribological properties of the steel-related friction system and the tribological properties of the friction pair are significantly influenced by lubrication modes and the types and contents of nano lubricant additives under PFPE oil lubrication. The friction system exhibits super low friction behaviors under PFPE oil with nano MoS₂ lubricant additive lubrication due to the excellent compatibility of nano MoS₂ additives with PFPE oil. Coefficient of friction (CoF) of the friction system is as super low as 0.02 under PFPE oil with 0.2?wt.% nano MoS₂ additive lubrication. Superlow friction mechanism is attributed to the pointlike contact of nano MoS₂ additive as soft phase and the excellent diffusion behaviors of nano MoS₂ additives in PFPE oil. The potential usefulness of nano MoS₂ particles as the lubricant additives in PFPE oil for the steel/DLC films has been demonstrated.     

Mechanical properties of DLC films prepared in acetylene and methane plasmas using electron cyclotron resonance microwave plasma chemical vapor deposition

Diamond-like carbon (DLC) films were deposited on silicon using methane and acetylene plasma induced by electron cyclotron resonance microwave plasma chemical vapor deposition (ECR-MPCVD). The mechanical properties of DLC films were characterized by micro-Raman system, atomic force microscope, tribometer, nano-indenter used for both hardness and nano-scratch test measurements. The mechanical properties of both DLC films, prepared in methane and acetylene plasmas, respectively, strongly depended on the kinetic energy of impinging particles. The deposition at −120 V substrate bias gave rise to DLC films with the best mechanical properties for both methane and acetylene plasmas. The hardness measurements with variable indentation depth showed the characteristic changes in hardness values implying elastic deformations of supporting substrates. The maximum hardness value of DLC^M films was 20 GPa while that of DLC^A films was 28 GPa. However, the hardness dropped when DLC films were prepared at substrate biases more negative than −120 V due to the thermal graphitization. The improvement in DLC properties usually provided the films with smaller hydrogen content and higher density of sp³ bondings. These parameters were engineered through controlling the deposition parameters. Particularly, the bombardment of growing DLC films by energetic ions showed to be extremely important to yield films with lower internal stress.     

Synthesis and Tribological Behavior of Silicon Oxycarbonitride Thin Films Derived from Poly(Urea)Methyl Vinyl Silazane

A process for deposition of silicon oxycarbonitride films from poly(urea)methyl vinyl silazane (PUMVS) by spin coating precursor solutions onto a substrate, followed by polymerization, cross-linking and pyrolysis has been developed. The cross-linked polymer films (350 nm thick), deposited on variety substrates (e.g., silicon, sapphire, zirconia), were pyrolyzed in nitrogen or ammonia environments either in a hot isostatic press or in a tube furnace. Their microstructure was characterized using infrared and Raman spectroscopy. The tribological (friction and wear) behavior was evaluated in dry nitrogen and air with 50% relative humidity using a unidirectional linear wear tester in a ball-on-disk configuration. Wear surfaces, transfer films and wear debris were analyzed by scanning electron micrograph (SEM)/energy dispersive spectroscopy (EDS).     

Tribological properties of DLC films with different hydrogen contents in water environment

Diamond-like carbon (DLC) films were deposited on silicon wafers by thermal electron excited chemical vapor deposition (CVD). To change the hydrogen content in film, we used three types of carbon source gas (C₇H₈, CH₄, and a CH₄+H₂) and two substrate bias voltages. The hydrogen content in DLC films was analyzed using elastic recoil detection analysis (ERDA). Tribological tests were conducted using a ball-on-plate reciprocating friction tester. The friction surface morphology of DLC films and mating balls was observed using optical microscopy and laser Raman spectroscopy.Hydrogen content in DLC films ranged from 25 to 45 at.%. In a water environment, the friction coefficient and specific wear rate of DLC films were 0.07 and in the range of 10⁻⁸–10⁻⁹ mm³/Nm, respectively. The friction coefficient and specific wear rate of DLC film in water were hardly affected by hydrogen content. The specific wear rate of DLC film with higher hardness was lower than that of film with low hardness. Mating ball wear was negligible and the friction surface features on the mating ball differed clearly between water and air environments, i.e., the friction surface on mating balls in water was covered with more transferred material than that in air.     

类金刚石薄膜在人工关节摩擦副表面改性进展

类金刚石（DLC）薄膜由于其优异的减摩耐磨性以及良好的生物相容性被引入到人工关节材质中。该文综述了DLC薄膜在人工关节摩擦副表面改性的研究现状，包括DLC薄膜的分类和制备方法。尽管该薄膜已被研究数十年，但在人体复杂的生理力学环境中高负荷摩擦腐蚀等综合作用下，仍存在高内应力导致结合力不足，从而限制其在人工关节领域的应用。该文介绍了降低DLC薄膜内应力提高膜基结合力的方法和DLC薄膜生物相容性的研究进展。最后，对不同DLC薄膜人工关节摩擦副的研究进展进行了阐述。根据该综述，提出厚的无氢DLC涂层（高sp3含量），且在两个滑动表面上均有DLC薄膜的人工关节副具有优异的耐磨性，对于承重植入体应用至关重要。     

Mechanical and tribological properties of diamond-like carbon coatings films deposited from an electron cyclotron resonance plasma

The friction coefficients have been investigated in amorphous diamond-like carbon (DLC) films deposited by a dual ECR–r.f. method, as a function of r.f. substrate bias in relation with the H content and bonding. Combined infrared absorption, elastic recoil detection analysis and tribological tests are used to characterize fully the films in their as-deposited state. Friction coefficients (μ) of the coatings against sapphire balls are determined in air at room temperature. The results indicate clearly that the samples exhibit high compressive stresses and the friction coefficients are found to be low and are affected by the magnitude of the biaxial stress and the microstructure of the films.     

硬质合金刀具类金刚石涂层的摩擦磨损性能

以等离子体化学气相沉积技术在硬质合金刀具表面制备了类金刚石(DLC)涂层.研究了DLC涂层刀具和无涂层刀具的硬度,不同载荷、不同转速下两种刀具的摩擦磨损性能,以及在水润滑和油润滑条件下DLC涂层刀具的滑动摩擦行为.结果表明,DLC涂层刀具的平均硬度为2 099.9 HV,比无涂层刀具提高了48.3%;DLC涂层刀具的摩擦因数明显低于无涂层刀具,其磨损率随着载荷的增加而增大,随转速的增大而减小;油润滑比水润滑能更有效减缓摩擦作用.     

Microstructure and adhesion characteristics of diamond-like carbon films deposited on steel substrates

For tribological applications, the low friction coefficient and high microhardness of diamond-like carbon (DLC) films give significant advantages in cutting and forming non-ferrous materials. The inherently large residual stress of DLC films, however, prevents the depositing of thicker films. This study designed and implemented a compound interface, comprising a series of metal, metal nitride, and metal carbonitride interlayers deposited in a graded structure, between the DLC (a metal-doped a-C:H) film and M2 steel substrates. The tribological performance of the interface was evaluated using a scratch tester and ball-on-disk tribometer. Meanwhile, the failure mechanism of DLC deposited on M2 steel substrates was examined using SEM/EDS and TEM microscopy. Experimental results demonstrate an improved DLC hard coating with superior adhesion strength on the steel substrates.     

A study of biotribological behavior of DLC coatings and its influence to human serum albumin

Diamond-like carbon (DLC) coatings has been synthesized on NiTi alloy substrates by arc enhanced magnetic sputtering (AEMS) system using graphite targets. The tribological behavior indicates that the friction coefficient and wear rate of DLC coatings deposited on NiTi alloy substrates is relatively higher in ambient air than that in simulated body fluid (SBF). In human serum albumin (HSA) solution, though the friction coefficient is higher than that in SBF, but it has quite low wear rate. The Raman spectrum shows that the low friction coefficient of DLC coatings is due to the graphitization during sliding, and the degree of graphitization is relatively lower in both SBF and HSA solution than them in ambient air. The friction mechanism of DLC coatings at different environments is then proposed. On the other hand, the kinematic viscosity and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) measurements show that the DLC coatings cannot induce the thermal and mechanical denaturation of HSA during sliding.     

Synthesis and Tribology of Carbide-Derived Carbon Films

Carbide-derived carbon (CDC) films are produced at atmospheric pressure on the surfaces of carbide-based ceramic materials and coatings by a high-temperature chlorination process. These nanoporous carbon films contain carbon nano-onions and amorphous carbon, and may contain nanocrystalline diamond and graphite as well, depending on the synthesis conditions. The combination of such diverse carbon phases in one material or coating provides unique and potentially useful properties for a wide range of engineering applications. In this paper, we will present the results of a comprehensive study on the tribological behavior of these films. The friction coefficient of CDC in open air is comparable with that of graphite and is typically in the range of 0.15–0.25. However, the friction coefficients of CDC tend to decrease with decreasing humidity. In dry nitrogen, its friction coefficient is ∼0.1 or less. Such behavior is in contrast to that of crystalline graphite, which normally exhibits low friction at high humidity, but high friction at low humidity or in vacuum. The friction coefficient of CDC becomes increasingly lower under heavier loads; however, increasing sliding velocity does not seem to affect its frictional behavior significantly. Using a hydrogenation process that removes residual chlorine from the CDC film, the friction coefficients of CDC can be further lowered to values as low as 0.03. In an attempt to understand some of the underlying mechanisms, we carried out comprehensive chemical and structural studies of the sliding surfaces as well as bulk films and correlated these findings with the friction and wear behavior of CDC films.     

Temperature Dependence of Diamondlike Carbon Film Tribological Characteristics

The tribological characteristics of a diamondlike carbon (DLC) film deposited on high-speed steel were investigated systematically by using a ball-on-flat reciprocating tribometer over a range of temperatures (from −40° to 20°C). The results indicated that the temperature dependence of the DLC film's tribological behavior was associated with the counterpart material. DLC presented favorable tribological behavior while sliding on itself. However, when a steel ball slides against the DLC film, there is evidence that the heat generated has a significant impact on friction and wear. Microanalysis of wear tracks on the films showed that multiple wear mechanisms took place during testing. At higher temperatures, material transfer dominated the wear behavior, while fatigue-induced microcracking was the predominant wear mechanism at low temperatures. Raman analysis indicated that the DLC film was mechanically worn rather than removed by tribochemical interactions between the friction pairs.     

Relation between physical structure and electrical properties of diamond-like carbon thin films

Diamond-like carbon (DLC) belongs to very interesting materials used for a number of practical applications. Its properties strongly depend on the method of deposition and on the deposition parameters. In particular, the electrical properties of DLC films obtained by RF PCVD discharge depend substantially on the preparation conditions. Influence of deposition conditions on the physical structure and chemical content is discussed. Both the drift mobility of charge carriers and the electrical conductivity of DLC films strongly depend on deposition conditions. The electrical conductivity results are explained in terms of hopping mechanism. At the temperatures below 260 K, the hopping among states in a narrow band of states dominates; at the higher temperatures, the band-to-band transitions are suggested to occur. A model of the forbidden gap explaining the observed electrical properties of DLC films is proposed. Experimental results concerning the electrical conduction of DLC/Si heterostructures are also presented and discussed. The difference in the properties of DLC/n-Si and DLC/p-Si structures may suggest that the electron transport via localised states dominate in the investigated DLC films. Recombination lifetime of charge carriers in DLC films is measured using both dielectric spectroscopy and detection of decay of photocurrents. The lifetime is found to be of the order of 0.3–0.4 ms, which is quite long in comparison with classical doped silicon semiconductors.     

Synergistic effect of surface textures and DLC coatings for enhancing friction and wear performances of Si3N4/TiC ceramic

To enhance the tribological properties of Si₃N₄ based ceramics, surface textures of dimples combined with DLC coatings are fabricated on Si₃N₄/TiC ceramic surface by nanosecond laser and plasma enhanced chemical vapor deposition (PECVD). The dry friction and wear performances are evaluated by unidirectional sliding friction tests using a rotary ball-on-disk tribometer. Results reveal that the friction and wear properties of Si₃N₄/TiC ceramics are significantly enhanced by DLC coatings or dimpled textures, and the DLC coatings combined with dimpled textures show the best efficiency in reducing friction, adhesion and wear. This improvement can be explained by the synergistic effect of DLC coatings and surface textures, and the synergistic mechanisms are attributed to the formation of lubrication film and secondary lubrication, debris capture of dimpled textures, increased surface hardness and mechanical interlocking effect, and reduced contact area.     

Chemical,mechanical and tribological characterization of ultra-thin and hard amorphous carbon coatings as thin as 3.5 nm: recent developments

Diamond material and its smooth coatings are used for very low wear and relatively low friction. Major limitations of the true diamond coatings are that they need to be deposited at high temperatures, can only be deposited on selected substrates, and require surface finishing. Hard amorphous carbon (a-C), commonly known as diamondlike carbon (DLC), coatings exhibit mechanical, thermal and optical properties close to that of diamond. These can be deposited with a large range of thicknesses by using a variety of deposition processes, on variety of substrates at or near room temperature. The coatings reproduce substrate topography avoiding the need of post finishing. Friction and wear properties of some DLC coatings can be very attractive for tribological applications. The largest industrial application of these coatings is in magnetic storage devices. Recent developments in the chemical, mechanical and tribological characterization of the ultra-thin coatings are reviewed in this paper. The prevailing atomic arrangement in the DLC coatings is amorphous or quasi-amorphous with small diamond (sp³), graphite (sp²) and other unidentifiable micro- or nanocrystallites. The mechanical and tribological properties of the DLC coatings are dependent upon the deposition technique. Thin coatings deposited by filtered cathodic arc, ion beam and ECR-CVD hold a promise for tribological applications. Coatings as thin as 5 nm in thickness provide wear protection.     

Strongly adherent Al2O3 coating on SS 316L: Optimization of plasma spray parameters and investigation of unique wear resistance behaviour under air and nitrogen environment

Plasma spray deposition of Al₂O₃ is a well-established technique for thick ceramic coatings on various substrates to shield them from corrosion and wear. Owing to its high hardness, aluminum oxide is known to protect stainless steel substrates from wear. However, the plasma process requires optimization for desired coating thickness and adhesion strength. It is also necessary to understand the sensitivity of friction and wear resistance of the deposited coating on exposed environment for evaluation of service life. The study offers comprehensive investigation on plasma process parameters for the development of strongly adherent aluminium oxide coatings on SS 316L substrate. Impact of environment like dry air and dry nitrogen on tribological properties of the coatings was also investigated. Dense adherent coatings of alumina could be deposited on SS 316L at a plasma power of 20 kW with an intermediate bond coat of NiCrAlY to enhance the adhesion properties. The effects of stand-off distance and bond coat thickness on adhesion strength were additionally examined. Further, the coatings were characterised for phase composition, microstructure, microhardness and wear resistance potential. Reciprocating wear tests of the coatings were carried out using ball on disc reciprocating tribometer at different loading conditions (5, 10 and 15 N) at constant (5 Hz) sliding frequency. Unlike the coefficient of friction (COF), wear volume was found to increase with an increase in normal load. These adherent coatings revealed promising properties for the applications where the tribological failure of SS 316L in dry air or dry nitrogen environment is to be controlled.