纳米结构碳基薄膜的制备及性能研究

利用单极脉冲等离子体增强化学气相沉积技术在单晶硅衬底上沉积含氢碳薄膜,用高分辨透射电子显微镜和激光拉曼光谱仪研究薄膜的微观结构,用X射线光电子能谱分析薄膜的化学键状态,并用纳米压痕仪测定薄膜的硬度和弹性模量,在CSM往复式摩擦磨损试验机上考察薄膜的摩擦学性能。结果表明:在单极脉冲等离子体增强化学气相沉积系统上成功制备出在非晶基体上镶嵌弯曲类富勒烯纳米结构的含氢碳薄膜,其独特的类富勒烯纳米结构赋予薄膜良好的力学性能,其弹性恢复系数和硬度分别高达86%和26.37 GPa;与非晶结构薄膜相比,制备的纳米结构含氢碳薄膜在室温环境下摩擦学性能更为优异,在机械摩擦表面具有广阔的应用前景。     

含氢类富勒烯碳薄膜制备及超滑性能研究进展

类富勒烯碳薄膜是一种由弯曲石墨烯镶嵌的非晶网络复合结构,正是由于这种弯曲石墨烯结构(类富勒烯结构)的存在,赋予了薄膜高的硬度,优异的弹性恢复和超低摩擦性能(摩擦因数为0. 002～0. 009)。综述含氢类富勒烯碳薄膜制备方法、纳米结构调控机制、超低摩擦学机制及后处理对薄膜摩擦学性能的影响;探讨含氢类富勒烯碳薄膜在汽车发动机方面的应用,指出其可有效降低发动机部件的摩擦磨损,有利于发动机的节能减排;总结氢类富勒烯碳薄膜未来工程应用的潜在挑战,指出类富勒烯碳薄膜虽在可控范围内具有超滑性能,但未来如何实现全工况范围超滑和固油复合超滑将是一个主要研究方向。     

温度对类富勒烯碳氮薄膜微观结构与摩擦学性能的影响

采用直流反应磁控溅射分别在200、250、300和350℃条件下沉积类富勒烯碳氮薄膜,利用X射线光电子能谱(XPS)和扫描电子显微镜(SEM)表征薄膜的微观结构形貌,采用薄膜综合性能测试仪以及通过大气球盘摩擦试验研究薄膜的力学性能及摩擦学性能。结果显示:制备的类富勒烯CN_x薄膜中存在sp~2C-C、sp~2N-C和sp~3C-N化学键;随着沉积温度的升高,薄膜的结构变得更加致密,硬度、弹性模量以及弹性恢复系数逐渐增大,摩擦因数和磨损率降低;沉积温度为350℃制备的薄膜摩擦因数和磨损率最低,表现出优异的耐磨损性能。     

中频磁控溅射法制备厚类金刚石碳膜

采用中频对靶磁控法在M2高速钢基片上合成了厚达6μm的含铬类金刚石碳(DLC)薄膜,初步考察了中频磁控溅射工艺参数、DLC薄膜的多层梯度结构及薄膜力学和摩擦性能间的关系。结果表明,薄膜表面平滑,具有致密的多层梯度结构,在2.45 N载荷下维氏硬度为HV 2 560,结合力的临界载荷为52 N,且在较长滑动距离内平均摩擦因数为0.09。     

离子束增强沉积Ni、Ti纳米金属薄膜的表面形貌与摩擦特性研究

在原子力显微镜上对采用离子束增强沉积方法制备的Ni、Ti纳米金属薄膜的形貌进行了观察,应用分形理论分析了薄膜表面的分形特征,并且对金属薄膜的纳米摩擦特性进行了研究,分析了载荷和表面力对金属薄膜摩擦特性的影响。结果表明,Ti薄膜晶粒细小,表面平整,而Ni薄膜表面粗糙。Ni、Ti沉积薄膜表面具有显著分形特征,各向同性。Ni、Ti纳米薄膜的摩擦力均随载荷的增大而增大,并且都存在一个临界载荷值,超过这个值,摩擦力急剧增加。将分形理论和接触力学JKR模型结合,对纳米金属薄膜摩擦的临界载荷进行的预测与实验结果具有相同的趋势。     

Ti-DLC薄膜在水介质中的摩擦学特性

采用非平衡磁控溅射法在Si(100)片和M2工具钢上制备Ti-DLC薄膜。通过X射线光电子能谱仪、拉曼光谱仪和扫描电子显微镜分析薄膜的结构以及微观形貌;利用球-盘摩擦磨损试验机研究不同载荷下Ti-DLC/Si-3N-4对摩副在水中的摩擦学特性。结果表明,Ti-DLC薄膜具有致密的表面结构,含有较多的C-Csp2键;摩擦介质为去离子水时,薄膜的摩擦因数随着载荷的增加先减小后增大,且载荷增加到一定值后,摩擦因数几乎不再变化; 薄膜磨损率随着载荷的增加先升高后降低,而相应的Si3N4小球磨损率却是先减小后增大, 这主要是由于Si3N4在水中易于发生水合反应,促使摩擦接触表面变得非常平滑,从起到降低摩擦因数,在一定程度上减少磨损的作用。     

类陨石坑表面类金刚石薄膜的制备及摩擦特性

为了提高DLC（Diamond-like Carbon）类金刚石薄膜与SAE1060碳素钢基材的结合强度,以延长发动机活塞环的使用寿命,研制了一种带有复合阳极的RF-DCCVD双电源化学气相沉积设备。利用锯齿结构的辅助阳极产生尖端放电,制备了具有微米类陨石坑非连续结构的DLC薄膜,并利用Ball-on-Disk摩擦评价试验机评价了薄膜的摩擦特性。着重研究了极间距S -T对薄膜表面类陨石坑密度的影响;最后利用拉曼光谱仪分析了薄膜结构和成分。结果表明：在同样的电压下,类陨石坑的密度随着电极间距的增加而减小,最佳电极间距S -T为40~60 mm,此时不仅具有比较适中的类陨石坑密度,对DLC薄膜的摩擦特性影响不大,而且具有较强的界面结合强度。当S-T为50 mm,施加载荷为3 N时,薄膜的破坏寿命达到了130万循环,比光滑表面的薄膜延长了30万循环。得到的结果显示微米类陨石坑非连续结构能够有效地释放膜内的残余压缩应力,延长SAE1060碳素钢基材上沉积类金刚石薄膜的使用寿命。     

类金刚石碳基薄膜在1-乙基-3-甲基咪唑四氟硼酸盐中的摩擦学性能

利用射频等离子体增强化学气相沉积技术,以甲烷为气源,在单晶硅(P(001))衬底上制备类金刚石碳基薄膜(DLC);利用高速往复摩擦磨损试验机分别测试DLC薄膜/Al2O3球摩擦副在大气环境下和1-乙基-3-甲基咪唑四氟硼酸盐离子液润滑下的摩擦磨损性能;利用光学显微镜,X射线光电子能谱和三维轮廓仪分别对磨痕、磨痕表面元素和磨损率进行考察。实验结果表明:DLC薄膜在离子液润滑时,在低载荷下减摩作用明显,但在较高载荷下摩擦因数较无离子液润滑时高,且不随载荷增加而变化,推测是离子液形成了边界润滑膜;XPS分析表明这层边界润滑膜可能是由离子液物理吸附在摩擦接触面上形成的,并且对DLC薄膜有很强的抗磨作用。     

氮化硅陶瓷表面DLC膜的制备及摩擦性能研究

利用等离子体基离子注入与沉积技术,在氮化硅陶瓷片表面制备200～400nm的类金刚石碳膜。测试薄膜的厚度、表面形貌、结构、膜基结合力,利用球盘试验机考察DLC膜的摩擦性能。结果表明:沉积薄膜均匀光滑;薄膜的硬度和弹性模量与基体差异较小,膜基结合力强;DLC膜具有较低的摩擦因数,抗磨性能优异。     

类金刚石薄膜微观摩擦性能的FFM评价——针尖尺度效应

采用等离子体增强气相沉积制备了类金刚石薄膜，利用原子力显微镜的轻敲模式观察了它们的形貌，并在考虑外加载荷和扫描速度的基础上，用摩擦力显微镜（FFM）对比考察了尖端探针和平头探针对类金刚石薄膜摩擦性能评价的影响。结果表明：类金刚石薄膜的表面粗糙度随基底负偏压的增加而减小；存在于探针和类金刚石薄膜之间的水膜对尖端探针的剪切阻力贡献较大，且尖端探针测得的摩擦力变化趋势受扫描速度影响显著；水膜对平头探针起着不同形式的润滑作用，从而导致平头探针和类金刚石薄膜之间摩擦性能的速度效应存在差异；利用摩擦力显微镜考察类金刚石薄膜的摩擦性能时，存在着明显的针尖尺寸效应。     

Ultralow Friction Behaviors of Hydrogenated Fullerene-Like Carbon Films: Effect of Normal Load and Surface Tribochemistry

Friction and wear behaviors of hydrogenated fullerene-like (H-FLC) carbon films sliding against Si₃N₄ ceramic balls were performed at different contact loads from 1 to 20 N on a reciprocating sliding tribometer in air. It was found that the films exhibited non-Amontonian friction behaviors, the coefficient of friction (COF) decreased with normal contact load increasing: the COF was ~0.112 at 1 N contact load, and deceased to ultralow value (~0.009) at 20 N load. The main mechanism responsible for low friction and wear under varying contact pressure is governed by hydrogenated carbon transfer film that formed and resided at the sliding interfaces. In addition, the unique fullerene-like structures induce well elastic property of the H-FLC films (elastic recovery 78%), which benefits the high load tolerance and induces the low wear rate in air condition. For the film with an ultralow COF of 0.009 tested under 20 N load in air, time of flight secondary ion mass spectrometry (ToF-SIMS) signals collected inside and outside the wear tracks indicated the presence of C₂H₃ ⁻ and C₂H₅ ⁻ fragments after tribological tests on the H-FLC films surface. We think that the tribochemistry and elastic property of the H-FLC films is responsible for the observed friction behaviors, the high load tolerance, and chemical inertness of hydrogenated carbon-containing transfer films instead of the graphitization of transfer films is responsible for the steady-state low coefficients of friction, wear, and interfacial shear stress.     

Superlow Friction of Diamond-Like Carbon Films: A Relation to Viscoplastic Properties

Composition, structure, electrical, optical, mechanical properties and tribological behavior of diamond-like carbon films (DLC) are strongly dependent on the deposition system. Some hydrogenated amorphous carbon films (a-C:H) may exhibit superlow friction properties in ultra-high vacuum (UHV). The present paper compares tribological and mechanical properties of several DLC films prepared under different conditions. Friction coefficients were measured in an analytical ultra-high vacuum tribometer. The mechanical properties were evaluated from force-displacement curves using a nanoindentation instrument. Making use of continuous stiffness mode, Young's modulus and hardness were determined as a function of indentation depth. The measurements were performed at constant strain rates by special control of the load during indentation. We were, thus, able to determine the dependence of hardness on strain rate, characterizing a viscoplastic behavior. Many of the hydrogenated amorphous carbon films studied were significantly viscoplastic. The aim of this paper is to highlight the correlation between superlow friction and viscoplastic behavior.     

沉积气压对W-S-C复合薄膜结构和摩擦学性能的影响

采用磁控溅射方法制备W-S-C复合薄膜,研究沉积气压对薄膜结构和摩擦学性能的影响。结果表明,复合膜以非晶或纳米晶结构生长,沉积气压低时薄膜中C含量高,薄膜结构致密;沉积气压高时薄膜中WSx含量高,薄膜致密性下降。复合膜硬度在HV420～500之间,并且随着沉积气压的增加,硬度逐渐下降。在潮湿大气中的摩擦磨损实验表明,实验载荷越大摩擦因数越小;随着沉积气压的增加,复合膜的摩擦因数先降低后增加;当沉积气压在0.45～0.55 Pa时,复合膜的摩擦因数最低约为0.1,耐磨性能最好。     

Friction of diamond-like carbon films in different atmospheres

Diamond-like carbon (DLC) films constitute a class of new materials with a wide range of compositions, properties, and performance. In particular, the tribological properties of these films are rather intriguing and can be strongly influenced by the test conditions and environment. In this paper, a series of model experiments are performed in high vacuum and with various added gases to elucidate the influence of different test environments on the tribological behavior of three DLC films. Specifically, the behavior of a hydrogen-free film produced by a cathodic arc process and two highly hydrogenated films produced by plasma-enhanced chemical-vapor deposition were studied. Flats and balls used in these experiments were coated with DLC and tested in a pin-on-disc machine under a load of 1 N and at constant rotational frequency. With a low background pressure, in the 10⁻⁶ Pa range, the highly hydrogenated films exhibited a friction coefficient of less than 0.01, whereas the hydrogen-free film gave a friction coefficient of approximately 0.6. Adding oxygen or hydrogen to the experimental environment changed the friction to some extent. However, admission of water vapor into the test chamber caused large changes: the friction coefficient decreased drastically for the hydrogen-free DLC film, whereas it increased slightly for one of the highly hydrogenated films. These results indicate that water molecules play a prominent role in the frictional behavior of DLC films—most notably for hydrogen-free films but also for highly hydrogenated films.     

Microtribological behaviour of thin DLC films using different testing methods

To enhance the lifetime and reliability of microcomponents, thin microtribological films are applied to microparts. With reduction of the component size, investigation methods for tribological testing must be adapted. This paper studies the microtribological behaviour of thin diamond‐like carbon (DLC) films using different testing methods. To tie in with macroscopic results, to determine friction we used the well‐known pin‐on‐disc test with spherical surfaces of 10 mm diameter under a typical load of 3 N. For investigations of the behaviour under single asperity contact, Atomic Force Microscope (AFM) methods with applied loads of a few hundred micronewtons were used. Investigations on thin DLC films showed that the friction coefficient under single asperity contact is strongly dependent on the applied load and the resulting contact area. Especially for thin films (up to a few hundred nanometres) the friction coefficient is influenced by the substrate material. With decreasing substrate Young's modulus the friction coefficient also decreases. On the other hand, an increase in the abrasive wear resistance was observed using soft substrate materials. In this paper we show that the friction coefficient was also reduced by a simple surface structure. For investigations we used photolithography to create concentric circles in different substrates. This resulted in a behaviour like riding on rails for the pin‐on‐disc test. Depending on the tribological pairing the friction coefficient was reduced to more than 50% of the original value. Copyright © 2006 John Wiley & Sons, Ltd.     

Tribological Performance of Diamond and Diamondlike Carbon Films at Elevated Temperatures

In this study, the authors investigated the tribological performance of diamond and diamondlike carbon (DLC) films as a function of temperature. Both films were deposited on silicon carbide (SiC) by microwave plasma chemical vapor deposition and ion-beam deposition processes. Tribological tests were performed on a reciprocating wear machine in open air (20 to 30% relative humidity) and under a 10 N load using SiC pins. For the test conditions explored, the steady-state friction coefficients of test pairs without a diamond or DLC film were 0.7 to 0.9 and the average wear rates of pins were 10^?5 to 10^?7 mm³/N·m, depending on ambient temperature. DLC films reduced the steady-slate friction coefficients of the test pairs by factors of three to five and the wear rates of pins by two to three orders of magnitude. Low friction coefficients were also obtained with the diamond films, but wear rates of the counterface pins were high due to the very abrasive nature of these films. The wear of SiC disks coated with either diamond or DLC films was virtually unmeasurable while the wear of uncoated disks was substantial. Test results showed that the DLC films could afford low friction up to about 300° C. At higher temperatures, the DLC films graphitized and were removed from the surface. The diamond films could withstand much higher tempera-lures, but their tribological behavior degraded. Raman spectroscopy and scanning electron microscopy were used to elucidate the friction and wear mechanisms of both films at high temperatures.     

Tribological Properties of Diamond-Like Carbon Films in Low and High Moist Air

Diamond-like carbon (DLC) film was deposited on Si wafer by a plasma CVD deposition system using benzene. Tribological properties of the DLC film were evaluated using a ball-on-disk tribo-meter in low (RH 1720 %) and high humidity (RH 9095 %) conditions in air. The effect of sliding speed (4.2 mm/s to 25 mm/s) and load (1.06 N to 3.08 N) on friction and wear was investigated. The friction behavior of the DLC film was obviously different in low and high humidity. When tested under low humidity conditions, the friction coefficient decreased significantly with increasing speed, and increased with load. However, under high humidity conditions, the friction coefficient increased with the speed and decreased with increasing load. The wear of the DLC film was little influenced by the sliding speed, normal load and humidity; a level of 10^-8 mm³/Nm could be obtained in all tests. The formation of a uniform transfer layer would be the main factor which controlled the friction coefficient of the DLC films. Unlike the friction, the wear resistance of the DLC film is not so easy to discuss and may be affected mainly by the tribo-chemical reaction in all the test conditions.     

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.     

Grey theory applied to evaluate the tribological performances of the a-C:H(N) coating films prepared by differing the nitrogen content and the film thickness

The purpose of this paper is to study the tribology performances of the aC:H(N) films by using a nanotester under different scratch loads and velocities. From the measurements of the friction coefficient and wear volume, the tribological performances including wear resistance and friction coefficients were evaluated for the hydrogenated amorphous carbon films prepared by differing film thickness and nitrogen volume friction in the gas mixture of (C₂H₂+N₂). Taguchi experimental design and the grey relational analysis were used to investigate the influence of specimen parameters (film’s thickness, nitrogen content in the film), and operating conditions in tribological tests (scratch load and scratch velocity) on the friction coefficients and the wear volume arising in the specimens with different coating films. It is found that the wear volume of thin film is increased by increasing either the nitrogen volume fraction or film thickness. Moreover, the optimal combination of the testing parameters was also determined in the use of the present model.     

Sliding friction and wear properties of CNX/TiN composite films

A combined dc magnetron sputtering and multi-arc deposition system was used to grow CN_X/TiN composite films on a high-speed-steel (HSS) substrate. The thickness of these films is about 3 μm, the hardness of the coating exceeds 50 GPa. The sliding friction properties were studied by ball-on-disc tests under different loads and speeds. The wear mode of the films was observed and analyzed. There exist spallation, abrasion and micro-ploughing wear modes under different loads. The critical load value was theoretically determined and tested to be 55 N. The results show that the alternating films have good wear resistance under heavy load and high speed.