Tribological Behavior of Multiply-Alkylated Cyclopentanes (MACs)-Cu Nanoparticles Composite Thin Film

Multiply-alkylated cyclopentanes (MACs) composite thin films containing Cu nanoparticles are fabricated on the octadecyltrichlorosilane (OTS)-modified substrate by a spin-coating technique. The thickness, wetting behavior, and nanoscale morphologies of the films are characterized by means of ellipsometry, contact angle measurement, and atomic force microscope (AFM). The friction and wear behaviors of the thin films sliding against Si₃N₄ ball are examined on a UMT-2MT tribometer in a ball-on-disk contact mode. The worn surfaces of the OTS-MAC-Cu composite film and the counterpart Si₃N₄ balls are investigated with a scanning electron microscope. Water contact angle on OTS-MAC-Cu composite film is higher than that of OTS-MAC film. OTS-MAC-Cu composite film exhibits higher load-carrying capacity and better friction reduction and antiwear behavior as compared with OTS-MAC film. This may be attributed to the load-carrying and self-repairing property of the Cu nanoparticles in the composite film and the formation of a transfer layer composed of OTS, MAC, and Cu on the rubbing surface of the counterpart ball.     

Friction,adhesion and wear durability of an ultra-thin perfluoropolyether-coated 3-glycidoxypropyltrimethoxy silane self-assembled monolayer on a Si surface

The tribological properties, such as coefficient of friction, adhesion and wear durability of an ultra-thin (<10?nm) dual-layer film on a silicon surface were investigated. The dual-layer film was prepared by dip-coating perfluoropolyether (PFPE), a liquid polymer lubricant, as the top layer onto a 3-glycidoxypropyltrimethoxy silane self-assembled monolayer (epoxy SAM)-coated Si substrate. PFPE contains hydroxyl groups at both ends of its backbone chain, while the SAM surface contains epoxy groups, which terminate at the surface. A combination of tests involving contact angle measurements, ellipsometry, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) was used to study the physical and chemical properties of the film. The coefficient of friction and wear durability of the film were investigated using a ball-on-disk tribometer (4?mm diameter Si₃N₄ ball as the counterface at a nominal contact pressure of ～330?MPa). AFM was used to investigate the adhesion forces between a sharp Si₃N₄ tip and the film. This dual-layer film had a very low coefficient of friction, adhesion and wear when compared to epoxy SAM-coated Si only or bare Si surface. The reasons for the improved tribological performance are explained in terms of the lubrication characteristics of PFPE molecules, low surface energy of PFPE, covalent bonding between PFPE and epoxy SAM coupled with reduced mobile PFPE. The low adhesion forces coupled with high wear durability show that the film has applications as a wear resistant and anti-stiction film for microcomponents made from Si.     

Improving the tribological performances of graphite-like carbon films on Si3N4 and SiC by using Si interlayers

Si interlayers were used to obtain the excellent tribological performances of graphite-like carbon (GLC) film on silicon nitride (Si₃N₄) and silicon carbide (SiC). The microstructure and mechanical characteristics of the as-prepared GLC films with Si interlayers were investigated by scanning electron microscopy, Raman spectroscopy, nanoindention and scratch test. The tribological behaviors of GLC-coated and uncoated Si₃N₄ and SiC were comparatively studied by a ball-on-disc tribo-meter in both dry and water environments. Results showed that the Si interlayers were dense and bonded well with both the substrates and GLC layers. The as-prepared GLC films exhibited excellent tribological performances in both dry and water environments. More importantly, the stably mild wear without any delamination was obtained in water by using Si interlayer. The mechanisms of friction reduction and anti-wear performances of GLC films on the two ceramics with Si interlayers under different environmental conditions were discussed, as well as the corresponding models were deduced.     

Characterization and tribological investigation of SiO2 and La2O3 sol–gel films

Thin films of SiO₂ and La₂O₃ were prepared on a glass substrate by a dip-coating process from specially formulated sols. The tribological properties of the resulting thin films sliding against a Si₃N₄ ball were evaluated on a one-way reciprocating friction and wear tester. The morphologies of the unworn and worn surfaces of the films were examined by an atomic force microscope (AFM) and a scanning electron microscope (SEM). La₂O₃ shows the best tribological performance. The coefficient of friction is about 0.1 and the wear life is over 5000 sliding passes both under higher (3 N) and lower load (1 N). The SiO₂ film derived from a specially formulated aqueous solution shows much better performance in resisting wear and reducing friction than the one derived from an ethanol solution. The wear mechanisms of the films are discussed based on SEM observation of the worn surface morphologies. SEM observation of the morphologies of worn surfaces indicates that the worn surface of La₂O₃ is too slight to be observed by SEM. The wear of SiO₂ derived from TEOS solution is the characteristic of delaminating, which is responsible for the abrupt failure of the film. The wear of SiO₂ derived from aqueous solution is the characteristic of fracture. Brittle fracture and severe abrasion dominate the wear of glass substrate.     

Formation of a protective film on a copper friction surface in the presence of fullerene C60

The influence of C₆₀ additive in industrial oil on the structure of the friction surface of copper foil in a steel-copper sliding friction pair is investigated by wide-angle x-ray diffraction, scanning electron microscopy, and hardness testing. The presence of C₆₀ in the lubricant leads to the formation of a thin film (of thickness <1000 Å) on the friction surface of the copper, where it protects the surface layers of the latter against major structural changes and helps to improve the tribological characteristics.     

Microstructure and tribological performance of self-lubricating diamond/tetrahedral amorphous carbon composite film

In order to smooth the rough surface and further improve the wear-resistance of coarse chemical vapor deposition diamond films, diamond/tetrahedral amorphous carbon composite films were synthesized by a two-step preparation technique including hot-filament chemical vapor deposition for polycrystalline diamond (PCD) and subsequent filtered cathodic vacuum arc growth for tetrahedral amorphous carbon (ta-C). The microstructure and tribological performance of the composite films were investigated by means of various characterization techniques. The results indicated that the composite films consisted of a thick well-grained diamond base layer with a thickness up to 150 μm and a thin covering ta-C layer with a thickness of about 0.3 μm, and sp³-C fraction up to 73.93%. Deposition of a smooth ta-C film on coarse polycrystalline diamond films was proved to be an effective tool to lower the surface roughness of the polycrystalline diamond film. The wear-resistance of the diamond film was also enhanced by the self-lubricating effect of the covering ta-C film due to graphitic phase transformation. Under dry pin-on-disk wear test against Si₃N₄ ball, the friction coefficients of the composite films were much lower than that of the single PCD film. An extremely low friction coefficient (∼0.05) was achieved for the PCD/ta-C composite film. Moreover, the addition of Ti interlayer between the ta-C and the PCD layers can further reduce the surface roughness of the composite film. The main wear mechanism of the composite films was abrasive wear.     

ECR-PECVD制备Si3N4薄膜的光学特性研究

本文研究了ECR-PECVD制备的Si₃N₄薄膜的光学特性.得到的Si₃N₄薄膜具有光致发光效应,在280℃沉积制备的Si₃N₄薄膜的光致发光波长为400nm,具有较好的单色性.测试分析了Si₃N₄薄膜对可见光、红外光具有较高的透射性能,Si₃N₄薄膜可作为红外光的增速减反射膜.     

Ti-Si-N复合膜的界面相研究

为了揭示Ti_Si_N复合膜中Si₃N₄界面相的存在方式及其对薄膜力学 性能的影响 ，采用x射线衍射仪、高分辨透射电子显微镜、俄歇电子能谱仪和显微硬度仪对比研究了磁 控溅射Ti_Si_N复合膜和TiN/Si₃N₄多层膜的微结构和力学性能. 实 验结果表明 ，Ti_Si_N复合膜均形成了Si₃N₄界面相包裹TiN纳米晶粒的微结构. 其中低Si 含量的Ti_Si_N复合膜中Si₃N₄界面相的厚度小于1nm，且以晶体态 存在，薄膜 呈现高硬度. 而高Si含量的Ti_Si_N复合膜中的Si₃N₄界面相以非晶 态存在，薄 膜的硬度也相应降低. 显然，Ti_Si_N复合膜中Si₃N₄界面相以晶体 态形式存在 是薄膜获得高硬度的重要微结构特征，其强化机制可能与多层膜的超硬效应是相同的. 关键词： Ti－Si－N复合膜 界面相 微结构 超硬效应     

Investigation of the running-in process and friction coefficient under the lubrication of ionic liquid/water mixture

The tribological properties of three different films commonly used in microelectromechanical systems (MEMS) under the lubrication of ionic liquid (IL)/water mixtures with various concentrations in the running-in process have been investigated. Results show that coefficients of friction (COFs) and wear rates for low temperature silicon oxide (LTO)/Si₃N₄ vary in a similar way to the ones for poly-Si/Si₃N₄ under the lubrications of different IL/water mixtures. In contrast, the differences in COFs and wear rates are more significant in that the COFs and wear rates increase dramatically with the decrease in IL/water concentration in the case of self-mated Si₃N₄, while the differences in COFs and wear rates for the two other tribopairs are relatively small when the concentration is changed. The period of the running-in process reduces with the increase in IL/water concentration for all the tribopairs. Effective hydrodynamic lubrication can be found in the case of Si₃N₄/Si₃N₄ tribopair at higher IL/water concentrations without an evident running-in process, however, such a phenomenon cannot be observed for the other two tribopairs. Different wear mechanisms will also be analyzed in this paper.     

The evolution of magnetic,electrical and structural properties of nanogranular [FeCoBN/SiN]×n thin films

Some results concerning the magnetic, electrical and microstructural properties of multilayer [FeCoBN/Si₃N₄]×n films in view of their utilization for manufacturing thin film magnetic inductors are presented. A comparison between the magnetic, electrical and structural properties of FeCoBN and [FeCoBN/Si₃N₄]×n thin films is also reported. The [FeCoBN/Si₃N₄]×n thin films with the thickness of the FeCoBN layers varied from 10 to 30 nm, exhibit good soft magnetic characteristics and high values for electrical resistivity such as Ms of 172–185 A m²/kg, Hc of 318–1433 A/m and ρ of 82–48×10⁻⁷ Ω m, respectively. These physical properties of the samples are discussed in relation with the microstructure of the multilayer system.     

Surface-modified Pd nanoparticles as a superior additive for lubrication

The tribological performance of lubricants is favourably altered by adding small amounts of nanoparticles which provide reduced wear and low friction. However, one of the main difficulties of using nanoparticles as additives is their dispersion or dissolution in lubricant oils, typically of hydrocarbon nature. With the surface modification of nanoparticles through long chain high molecular weight hydrocarbons, stable dispersions in lubricant oils become feasible. Here we show that using surface-modified Pd nanoparticles (2 nm size) with tetraalkylammonium chains, stable dispersions in lubricant oils become feasible with excellent tribological properties (friction 0.07, wear resistance 10⁻¹⁰ mm³/Nm). Electrical contact measurements were also used to monitor the conductivity of the contact during sliding. The use of these nanoparticles made decrease the electrical resistance of the contact a percentage of 97 to 99.5% in comparison with the initial value measured for the base oil alone. To understand these phenomena the contact surfaces and Pd nanoparticles were studied after friction by scanning electron microscopy (SEM) combined with energy dispersive X-ray analysis (EDX) and transmission electron microscopy (TEM), respectively. The outstanding performance is attributed to a combination of factors as metallic character of palladium, nanometric size, and replenishment of Pd nanoparticles onto the contact forming a transfer layer. This discovery opens new perspectives of using metallic nanoparticles as lubricant additives for small contacts and connectors applications.     

Structural and tribological properties of nitrogen doped amorphous carbon thin films synthesized by CFUBM sputtering method for protective coatings

Nitrogen doped amorphous carbon (a-C:N) films are a material that may successfully compete with DLC coatings, which have high hardness, high wear resistance, and a low friction coefficient. The a-C:N films were prepared on silicon substrate by a closed-field unbalanced magnetron sputtering method with a graphite target and using the Ar/N₂ mixture gases. And, we investigated the effects of various DC bias voltages from 0 to −300 V on the structural and tribological properties of the a-C:N films. This study was focused on improving physical properties of the a-C:N film by controlling process parameters like negative substrate DC bias voltage. The maximum hardness of the a-C:N film was 23 GPa, the friction coefficient was 0.08, and the critical load was 25 N on a Si wafer. Consequently, the structural and tribological properties of the a-C:N film showed a clear dependence on the energy of ions bombardment and the density of the sputtering and the reaction gases during film growth.     

From nitride to carbide: control of zirconium-based hard materials film growth and their characterization

High-quality thin films of ZrC_yN_1-y and the novel tribological material Zr_0.8Al_0.2C_yN_1-y have been grown by pulsed reactive crossed-beam laser ablation using Zr and Zr–Al ablation targets, respectively, and a pulsed gas. The gas mixture provided the carbon and nitrogen for the solid-solution films. Control of the stoichiometry (i.e. y) was determined by the relative partial pressures of the nitrogen- and carbon-containing gases. It was found that optimal control of the film chemistry was achieved by using the least thermally reactive gases. In this manner, it was possible to activate the gas species exclusively by collisions in the gas phase with the ablation-plume particles, thereby decoupling the chemistry from surface processes. The films were characterized for their chemical, crystallographic, optical, and tribological properties. All the films had very low impurity levels and a cubic rock salt crystal structure over the entire investigated temperature range between 100 and 600 °C. Exceedingly high quality epitaxial films could be grown on MgO (001) at 600 °C. Films grown on stainless steel were polycrystalline. The hardness of the films showed a maximum for both sets for stoichiometries predicted by a recent theoretical model for hardness based on band-structure calculations. In addition, all the films had an exceptionally low coefficient of friction versus steel. Received: 22 August 2001 / Accepted: 3 March 2002 / Published online: 19 July 2002     

Influence of magnetic powders on the tribological performance of a novel magnetic brake material

By adding magnetic powders into matrix material, it has been proved to be a creative approach to improve tribological properties of brake materials. In this paper, a novel magnetic brake material with Nd–Fe–B and nano-Fe₃O₄ was developed, and the influential mechanism of these two magnetic powders and their content on the friction and wear performance was deeply discussed. Firstly, some experiments were carried out to investigate the tribological performance and influential mechanisms of four groups of brake pad samples with different magnetic powders. Furthermore, based on these results, further experiments for investigating the influence that Nd–Fe–B contents have on the tribological properties were conducted. According to the theoretical analysis about experiments, it was concluded that nano-Fe₃O₄ is beneficial to promote the formation of friction film and has certain lubricant effects. However, Nd–Fe–B has double effects on the formation of friction film. It will have positive effects when its content is less than a certain value. Otherwise, it will destroy the structure of friction film. Conclusively, it is believed that this study will be significantly valuable and meaningful for developing new brake materials and improving safety reliability of mechanical brakes.     

Suppress polystyrene thin film dewetting by modifying substrate surface with aminopropyltriethoxysilane

Aminofunctional organosilanes, such as 3-aminopropyltriethoxysilane (APTES), have been widely utilized as adhesion promoters, and have also been found to have the ability to prevent dewetting of polymer thin films from substrates. The APTES molecule contains an active terminal amino group that can hydrogen bond with the multiple hydroxylated head groups in itself and hydroxyl groups on a substrate, thus forming cyclic structures and a complex loose network at ambient conditions. Upon heating, the hydrogen bond can be broken, allowing more silanol groups to condense with each other and form siloxane linkages, hence tightening the three-dimensional network. When a polymer thin film is in contact with the APTES layer during the thermal process, the polymer chains can diffuse/penetrate into the APTES network while the network is being tightened by the additional crosslinking. The penetrated and subsequently anchored chains could help to stabilize the thin film on the substrate. This hypothesis was verified by dewetting studies of thin films of polystyrene (PS), having molecular weights above and below the entanglement molecular weight (M_e), from APTES and control surfaces when the systems were subjected to various treatments. Dewetting suppression was observed for PS/APTES that was thermally treated at ∼80 °C or 120 °C prior to the annealing of the thin film at higher temperatures. Much stronger suppression was noticed for PS having a molecular weight higher than M_e. When PS thin films were deposited onto a precured APTES network, no dewetting suppression was observed.     

Crystal structure and tribological properties of molybdenum disulfide films prepared by magnetron sputtering technology

Molybdenum disulfide (MoS₂) is widely used in practice due to its excellent lubricating properties. However, research on the tribological properties of magnetron sputtering for depositing MoS₂ films remains limited. Herein, the tribological properties of MoS₂ films were investigated in detail through a series of characterization and friction coefficient tests. MoS₂ films were deposited onto silicon substrates by magnetron sputtering under different radio-frequency powers (P_rf). With increased P_rf, the crystallinity of the films gradually increases, whereas the friction coefficient initially decreases and then increases. P_rf also affects the chemical composition, surface morphology, and grain size of MoS₂ films. At P_rf = 300 W, the film surface is dense and smooth, the grain distribution is uniform. Moreover, the films have superior tribological properties and low friction coefficient, which can be attributed to the weak van der Waals force among MoS₂ layers and the microscopic morphology of the films. All these results indicate that by reasonably controlling the preparation parameters, MoS₂ films with excellent tribological properties can be prepared by magnetron sputtering.     

INVESTIGATION ON THE COMPOSITION AND STRUCTURE OF SILICON NITRIDE FILM PREPARED BY ECR-PECVD

In this paper, the effect of temperature on the composition and structure of the Si₃N₄ thin film is investigated. X-ray diffraction pattern and transmission electron microscope (TEM) analyses show that the Si₃N₄ film undergoes the transition from amorphous to crystalline phase with increasing deposition temperature. Infra-red qualitative analysis shows that the content of hydrogen decreases with increasing deposition temperature.The stoichiometric of Si₃N₄ is investigated by X-ray photoelectron spectroscopy or electron spectroscopy for chemical analysis.     

(Zr,V)N复合膜的结构、力学性能及摩擦性能研究

通过非平衡磁控溅射的方法制备了不同V含量的(Zr,V)N复合薄膜, 采用EDS, XRD, XPS, 纳米压痕仪和摩擦磨损仪等对薄膜的化学成分、微结构、力学性能及摩擦性能进行了研究. 结果表明, V的加入虽未改变ZrN的fcc晶体结构, 但使薄膜的择优取向由ZrN的(200)面转变为(Zr,V)N的(111)面. 随着V含量增加, (Zr,V)N复合膜的硬度略有升高后缓慢降低, 并在含25.8 at.%V后迅速降低. 与此同时, 薄膜的常温摩擦系数亦有小幅降低. 高温摩擦研究表明, (Zr,V)N薄膜在300 ℃时出现V₂O₃, V₂O₅ 在500 ℃后形成, 其含量也随温度的提高而增加. 薄膜的摩擦系数因V₂O₅ 的形成而得到显著降低. 关键词： (Zr,V)N 薄膜 微结构 力学性能 摩擦性能     

Microstructure and tribological behavior of pulsed laser deposited a-CNx films

The a-CN_x films were deposited onto high-speed steel substrate by pulsed laser deposition at different nitrogen pressures. The tribological properties of the films in humid air and in vacuum were investigated using a ball-on-disk tribometer under various loads. The composition, microstructure and morphology of the films, wear tracks and paired balls were characterized by energy dispersive X-ray analysis (EDXA), X-ray photoelectron spectrum (XPS), Raman spectroscopy and scanning electron microscopy (SEM). With increasing the deposition pressure, the fraction of sp³ C bond reduces, the fraction of trapped nitrogen increases and the friction coefficient of the films declines both in humid air and vacuum. The friction coefficient of a-CN_x film decreases with increasing normal load. The tribological performances of the films in humid air are better than those of in vacuum. A transferred graphite-like tribo-layer is observed from a-CN_x film to the paired ball for both environments.     

Mechanical properties of Ti(C0.7N0.3) film produced by plasma electrolytic carbonitriding of Ti6Al4V alloy

Porous nanocrystalline Ti(C_0.7N_0.3) film on Ti6Al4V substrate was prepared by plasma electrolytic carbonitriding (PECN). The film was characterized and analyzed by using a variety of analytical techniques, such as XRD, SEM, EDX, TEM, FESEM, Rockwell C indenter, scratch tester, Vickers microhardness tester and ring-on-block tribometer. The results showed that the film was about 15 μm thick and its hardness was Hv 2369 at a load of 0.2 N. The adhesion of the film was characterized by Lc and Pc value, and was found to be about 42 N and more than 800 N, respectively. The friction coefficients and wear volume loss of the PECN-treated samples sliding against a steel counterpart were much less than those of the untreated Ti6Al4V. The film possessed a good wear-resistance and antifriction under oil-lubricated condition due to its high hardness, adhesion and fracture toughness. Also, the porous surface morphology of the Ti(C_0.7N_0.3) film contributed to the enhanced tribological resistance by promoting the formation of lubricant film and entrapping wear debris.