氮气流量对磁控溅射制备类金刚石薄膜性能的影响

采用磁控溅射法以石墨为靶材在玻璃衬底上沉积了类金刚石(DLC)薄膜,用原子力显微镜表征了不同氮气流量条件下生长薄膜的形貌,用拉曼光谱仪、X射线光电子能谱仪和分光光度计分析了样品的微结构、元素的价态和透光性能.结果表明:沉积的薄膜均为非晶结构.通入2sccm氮气时,薄膜的光学透过率大大提高,此时DLC薄膜内的氮元素含量为5.88%,sp3键百分比为64.65%,ID/IG值为1.81;掺氮DLC薄膜在可见光范围内光学透过率达到95.69%.随着氮气流量增加,DLC薄膜光学透过率呈现出下降的趋势.退火2h后不掺氮DLC薄膜光学透过率呈小幅度下降,而掺氮DLC薄膜的光学透过率几乎没有变化.     

不同基底石墨烯涂层的层间滑移减磨性能研究

石墨烯薄膜作为一种二维材料,是提高微/纳机电系统(MEMS/NEMS)摩擦力学性能的优异润滑剂.为了探究基底材料和石墨烯层数对其减磨性能的影响,本文通过在不同基底制备了不同层数的石墨烯涂层,利用原子力显微镜(AFM)实验和分子动力学(MD)仿真结合的方法,研究了石墨烯层数对减磨效应的影响.并且通过建立不同层数石墨烯涂层的摩擦性能分析模型,探究出石墨烯层间滑移是产生减磨的主要因素.结果表明:在不同载荷下,石墨烯涂层对硅基底和铜基底均有优异的减磨效果,摩擦力随着石墨烯层数的增加逐渐降低,当石墨烯层数大于10层时,达到最优99.3%的减磨效果.通过仿真分析发现,随着层数增加,石墨烯与基底的干摩擦转变为石墨烯的层间摩擦,并产生层间剪切滑移,石墨烯层间滑移是导致多层石墨烯优异减磨性能的主要因素.     

涂覆聚甲基丙酸甲酯的磁性膜外磁场作用下的往复滑动摩擦行为研究

磁性材料被广泛应用于磁记录和磁润滑等领域,聚甲基丙烯酸甲酯因其良好的介电性,能够用作磁性材料的表面涂层.本文对外磁场作用下,外加载荷和磁场强度对往复滑动的聚甲基丙烯酸甲酯/磁性薄膜双膜系摩擦性能的影响开展了研究.实验结果表明:聚甲基丙烯酸甲酯/磁性双膜体系的摩擦性能随载荷和磁场强度改变而变化;但在干摩擦和硅油润滑两种模式下,磁场对其摩擦学性能的影响规律不同.理论分析了磁场作用下磁场诱发的磁性力与摩擦副物理性质变化对摩擦力和摩擦系数的影响,与实验结果符合良好.研究结果为磁性薄膜的界面介质设计与控制提供了依据.     

RF-PECVD法制备大面积类金刚石薄膜性能的研究

采用RF-PECVD法在锗、硅红外光学窗口上制备了大面积(基底直径φ=150～250mm)类金刚石薄膜.采用拉曼光谱分析了大面积DLC膜的结构组成,对RF-PECVD法制备的大面积DLC膜的均匀性、红外光学性能、机械力学性能以及其抗恶劣环境的能力进行了检测和分析.膜层厚度均匀性在3%以内.锗、硅红外窗口双面镀制DLC膜后,极值透过率分别达92%和96%以上,可显著提高红外光学窗口的显微硬度.膜层具有极强的抗盐雾、耐海水腐蚀和抗摩擦的能力.     

掺硅类金刚石膜的制备与力学性能研究

用脉冲电弧离子镀技术,通过调整掺硅石墨靶和纯石墨靶的数量,制备了一系列不同硅含量的类金刚石薄膜样品.研究发现：当硅含量达6.7at.%时,类金刚石薄膜的应力从4.5GPa降低到3.1GPa,薄膜的硬度还保持在3600Hv,和没有掺杂的类金刚石薄膜的硬度相比,基本保持不变;当硅含量小于6.7at.％时薄膜的摩擦系数相对于未掺杂的类金刚石薄膜也保持不变,为0.15.当薄膜中硅含量继续增加时,薄膜中C—Si键的含量增多,导致薄膜硬度和应力都有较大幅度地减小、摩擦系数增大、磨损性能也变差了. 关键词： 类金刚石膜 掺硅 应力 硬度     

纳米摩擦中极性有机分子超薄膜的结构、对称性及能量机理

采用分子动力学方法, 模拟了由脂肪酸C_nH_2n+1COOH和C₁₇H₃₅COOH (n=12,13,14,15,16,17) 按1:1比例组成的7种混合单层Langmuir-Blodgett (LB)膜和由C₁₆H₃₃COOH 分子组成的单层膜的摩擦性质. 结果显示: 1) 随着混合单层膜内的不同分子链长差的减小, 其剪切压随之减小, 摩擦力主要来自单层膜间的库伦作用; 2) 混合膜内的两种不同分子的尾基排列对其摩擦性能影响较大, 当混合LB膜中所有分子尾基全同排列时剪切压较小. 当分子链长差为1 个C-C键长时, 分子尾基排列对膜的摩擦性质影响较大. 3) 同种分子尾基全同排列组成的单层膜, 当上下两单层膜的尾基呈镜面对称时, 其剪切压随着分子链长的增加而减小, 摩擦力主要来自膜间的库伦作用; 当上下两单层膜的尾基呈中心对称时, 膜间摩擦力主要来自膜间的范德华 (VDW) 作用. 关键词： 分子动力学模拟 纳米摩擦 薄膜 库伦能     

一种适合微条气体室探测器的理想衬底材料

微条气体室(Micro-strip Gas Chamber,MSGC)探测器最严重的问题是电荷积累效应,通过选择合适的衬底材料可以有效的避免.为此,D263玻璃上沉积类金刚石(Diamond-like Carbon,DLC)膜来进行表面改性,从而制备DLC膜D/263玻璃双层结构作为MSGC衬底.拉曼光谱说明DLC膜是由sp³(σ键)和sp²(π键)杂化碳原子组成,属于电子导电型材料,并且沉积出的是一种高质量的DLC膜;I V曲线表明DLC膜改性后的样品具有非常稳定和理想的电阻率,其值在10⁹—10¹²Ω·cm间;C-F曲线显示改性后样品具有小而稳定的电容.DLC膜D/263玻璃的优良性能正是MSGC衬底的最佳要求,这种新型材料用作衬底将有效克服电荷积累效应和衬底不稳定性.     

微米级超润滑石墨接触面的表征与分析

超润滑可能是解决摩擦磨损问题的理想方案.目前已经能够在大气环境下实现基于石墨的微米尺度超润滑,但石墨接触面在超润滑实现过程中的影响还需要深入研究.为此,本文用电子束曝光及反应离子刻蚀方法在高定向热解石墨上加工出微米尺度的氧化硅/石墨方台结构,并用钨针尖推开方台的上部获得超润滑的石墨接触面.然后用原子力显微镜对多个石墨接触面进行了形貌表征,并使用能谱仪及X射线光电子能谱对石墨接触面的边缘进行测试.研究发现,高定向热解石墨的多晶结构在接触面的形成过程中有重要影响,能够决定接触面的质量进而决定超润滑能否实现.石墨接触面的边缘存在大量加工中引入的化学键及在大气中吸附的物理键,这些键是推开石墨方台形成接触面时阻力的来源,并在接触面发生相对滑动时表现为摩擦力.本文通过对具有微米尺寸的超润滑石墨接触面进行研究,明确了接触面内部及边缘影响超润滑实现的规律,对大面积超润滑的实现及应用能够提供有益的帮助.     

直拉硅单晶的机械强度:锗和氮共掺杂的效应

作为集成电路(ICs)的基础材料,直拉硅(CZ-Si)单晶的机械强度不仅是硅片加工和ICs制造过程中工艺参数设定的重要考虑因素,而且在很大程度上决定了ICs芯片在测试和封装过程中出现的失效情况.目前,ICs的器件特征尺寸仍在继续减小,由此带来的器件集成规模的增长会导致硅衬底中应力水平的提高,从而使位错更易产生.因此,改善直拉硅片的机械强度对于提高ICs的制造成品率具有重要意义.本文提出在直拉硅单晶中同时掺入锗和氮两种杂质来改善硅片机械强度的思路.基于此,对比研究了普通的、单一掺锗的、单一掺氮的、锗和氮共掺的直拉硅单晶的室温硬度及其在600—1200℃时的位错滑移行为.研究结果表明:1)单一的锗掺杂或氮掺杂以及锗和氮两种杂质的共掺几乎都不影响直拉硅单晶的室温硬度,意味着上述掺杂没有改变室温下的位错滑移行为. 2)氮掺杂能显著抑制位错在600—1000℃的滑移,但对位错在1100℃及以上温度的滑移几乎没有抑制效应;锗掺杂几乎不能抑制位错在600—900℃的滑移,但对位错在1000℃及以上温度的滑移具有显著的抑制效应. 3)锗和氮两种杂质的共掺对位错在600—1200℃的滑移均有显著的抑制效应,表明氮掺杂和锗掺杂的互补优势得到了很好的结合.分析认为,在600—1000℃的温度范围内,氮掺杂导致在位错核心处形成与氮-氧复合体相关的钉扎中心,从而抑制位错的滑移;在1000℃及以上温度,锗掺杂导致在位错前沿附近形成锗-氧复合体,从而阻碍位错的滑移.总之,本文的研究表明在直拉硅单晶中同时掺入锗和氮两种杂质可以进一步地增强硅片在ICs制造工艺温度下的机械强度.     

非平衡磁控溅射法制备的Cr-DLC薄膜真空退火的Raman光谱研究

利用非平衡磁控溅射法制得厚度达到2.23 μm的掺铬含氢类金刚石(Cr-DLC)碳膜。采用Raman光谱和XPS对制得的薄膜进行了结构和热稳定性等表征。结果表明：室温时,薄膜在1 544 cm-1附近的Raman“G”峰归属于石墨结构中C—C键的伸缩振动,即E_2g 模式;而1 367 cm-1附近的“D”峰归属于sp2碳环的“呼吸”振动模式,即A_1g模式;计算得到薄膜sp3键的相对含量约为48at.%。加热至300 ℃,薄膜的Raman谱图与室温时相似,表明此温度段薄膜的结构稳定,未发生明显改变;至400 ℃时,I_D/I_G值迅速增大,sp2键含量升高, 表明此时DLC膜发生了明显的结构变化,开始发生石墨化。继续升温,膜中I_D/I_G比率增加,“G”峰位向高波数方向位移,表明 sp2/sp3比率逐渐增大,薄膜石墨化程度加强,sp2键的无序度逐渐降低,最终导致薄膜的摩擦系数和磨损率等逐渐增大, 热稳定性逐渐降低。退火600 ℃时,I_D/I_G值以及sp2键含量达到最大值,DLC薄膜失效。     

Influence of sulfidation treatment on the structure and tribological properties of nitrogen-doped diamond-like carbon films

The nitrogen-doped diamond-like carbon (DLC) films were deposited on high speed steel (HSS) substrates in the direct current unbalanced magnetron sputtering system. Sulphurized layer was formed on the surface of DLC films by means of liquid sulfidation in the intermixture of urea and thiourea solution in order to improve the tribological properties of DLC films. The influence of sulfidation treatment on the structure and tribological properties of DLC films was investigated in this work. The structure and wear surface morphology of DLC films were analyzed by Raman spectroscopy, XPS and SEM, respectively. It reveals that the treated films are smooth and uniform; and sulfur atoms are bonded chemically. The treated films have broader distribution of Raman spectra in the range of 1000-1800 cm⁻¹ and higher I_D/I_G ratio than the untreated films as a result of the appearance of the crystalline graphite structure after the sulfidation treatment. It is showed that the sp² relative content increase in the treated films from the XPS measurement. The Raman results are consistent with the XPS results. The tribological properties of DLC films were investigated using a ball-on-disk rotating friction and wear tester under dry friction conditions. It is found that the sulfidation concentration plays an important part in the tribological properties of the treated DLC films. The results showed the treated films with low sulfidation concentration have a lower friction coefficient (0.1) than the treated films with high sulfidation concentration (0.26) and the untreated films (0.27) under the same friction testing conditions, which can be attributed to both the presence of sulfur-containing materials and the forming of the mechanical alloyed layer on the wear surface. Adding the dry nitrogen to the sliding surface in the testing system helps the friction coefficient of the treated films with low sulfidation concentration to decrease to 0.04 further in this work. On the basis of the experimental results, it is indicated that the liquid sulfidation technique, which is low-cost, non-polluting and convenience, would be an appropriate method for the surface treatment of DLC films.     

Study on tribological behavior and cutting performance of CVD diamond and DLC films on Co-cemented tungsten carbide substrates

The tribological behaviors of diamond and diamond-like carbon (DLC) films play a major role on their machining and mechanical applications. In this study, diamond and diamond-like carbon (DLC) films are deposited on the cobalt cemented tungsten carbide (WC-Co) substrate respectively adopting the hot filament chemical vapor deposition (HFCVD) technique and the vacuum arc discharge with a graphite cathode, and their friction properties are evaluated on a reciprocating ball-on-plate tribometer with counterfaces of silicon nitride (Si₃N₄) ceramic, cemented tungsten carbide (WC) and ball-bearing steel materials, under the ambient air without lubricating condition. Moreover, to evaluate their cutting performance, comparative turning tests are conducted using the uncoated WC-Co and as-fabricated CVD diamond and DLC coated inserts, with glass fiber reinforced plastics (GFRP) composite materials as the workpiece. The as-deposited HFCVD diamond and DLC films are characterized with energy-dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), X-ray diffraction spectroscopy (XRD), Raman spectroscopy and 3D surface topography based on white-light interferometry. Furthermore, Rocwell C indentation tests are conducted to evaluate the adhesion of HFCVD diamond and DLC films grown onto WC-Co substrates. SEM and 3D surface topography based on white-light interferometry are also used to investigate the worn region on the surfaces of diamond and DLC films. The friction tests suggest that the obtained friction coefficient curves that of various contacts exhibit similar evolution tendency. For a given counterface, DLC films present lower stable friction coefficients than HFCVD diamond films under the same sliding conditions. The cutting tests results indicate that flank wear of the HFCVD diamond coated insert is lower than that of DLC coated insert before diamond films peeling off.     

Friction and wear of rare earths modified carbon fibers filled PTFE composite under dry sliding condition

Carbon fibers (CF) were surface treated with air-oxidation and rare earths (RE), respectively. The friction and wear properties of polytetrafluoroethylene (PTFE) composites filled with differently surface treated carbon fibers, sliding against GCr15 steel under dry sliding condition, were investigated on a block-on-ring M-2000 tribometer. Experimental results revealed that RE treatment largely reduced the friction and wear of CF reinforced PTFE (CF/PTFE) composites. The RE treated composite exhibited the lowest friction and wear under dry sliding. Scanning electron microscopy (SEM) investigation of worn surfaces and transfer films of CF/PTFE composites showed that RE treated CF/PTFE composites had the smoothest worn surface under given load and sliding speed, and a continuous and uniform transfer film formed on the counterface. X-ray photoelectron spectroscopy (XPS) study of carbon fiber surface showed that the oxygen concentration was obviously increased after RE treatment, and more carboxyl groups were introduced onto CF surfaces after RE treatment. The increase in the amount of oxygen-containing groups increased the interfacial adhesion between CF and PTFE matrix, and accordingly increased the tribological properties of the composite.     

Preparation and tribological properties of DLC/Ti filmby pulsed laser arc deposition

This paper reports that DLC (diamond like carbon)/Ti and DLC films were prepared by using pulsed laser arc deposition. R-ray diffraction, Auger electron spectroscopy, Raman spectroscopy, atomic force microscopy, nanoindenter, spectroscopic ellipsometer, surface profiler and micro-tribometer were employed to study the structure and tribological properties of DLC/Ti and DLC films. The results show that DLC/Ti film, with $I(D)/I(G)$ 0.28 and corresponding to 76{\%} sp$^{3}$ content calculated by Raman spectroscopy, uniform chemical composition along depth direction, 98 at{\%} content of carbon, hardness 8.2 GPa and Young's modulus 110.5 GPa, compressive stress 6.579 GPa, thickness 46~nm, coefficient of friction 0.08, and critical load 95mN, exhibits excellent mechanical and tribological properties.     

Tribological effect of iron oxide residual on the DLC film surface under seawater and saline solutions

This paper discusses the seawater and saline solutions effects on the tribological behavior of diamond-like carbon (DLC) films. The adsorption of Fe on DLC surface is one of the mechanisms that is believed to be the cause of the decrease in dispersive component of the surface energy and increase of the I_D/I_G ratio leading to low friction coefficient and wear rate under corrosive environments. Tribological behaviors DLC films were experimentally evaluated under corrosive environments by using steel ball and DLC coated steel flat under rotational sliding conditions. The DLC films were prepared on 440 stainless steel disks by DC-pulsed PECVD using methane as a precursor gas. Two different set of tribological system was assembled, one when the liquids and the pairs were put inside of a stainless steel vessel and others inside of a PTFE. Every tribological test was performed under 10 N normal load120 mms^? 1 of sliding speed. The friction coefficients were evaluated during 1000 cycles.     

Tribological behavior of diamond-like carbon film with different tribo-pairs: A size effect study

A friction force microscope (FFM) with different probes and a ball-on-disk (BOD) tribo-meter were used to investigate the tribological properties of diamond-like carbon (DLC) films. DLC films were prepared by chemical vapor deposition (CVD) method by altering the deposition parameters, and their morphologies and structural information were examined with an atomic force microscope (AFM) and the Raman spectrum. The wear traces of the DLC films after frictional tests were analyzed by an optical microscope. It is found that surface roughness and adhesion play important roles in characterizing the tribological properties of DLC films using FFM. Moreover, the debris accumulation is another significant factor affecting the frictional behavior of DLC films, especially for the sharp tip. The difference in coefficients of friction (COFs) obtained by the BOD method among different DLC films under water lubrication is much smaller than the case without water lubrication. The variation trends in COF for the flat tip and the BOD test are similar in comparison with the result obtained with the sharp tip. The wear traces after frictional tests suggest that DLC films under water lubrication are prone to be damaged more readily.     

Influence of crystalline diamond nanoparticles on diamond-like carbon friction behavior

Crystalline diamond (CD) particles have been incorporated in diamond-like carbon (DLC) film structure in order to improve DLC electrochemical corrosion resistance. This paper shows the investigation of CD-DLC friction behavior according to the CD average sizes and concentration. The films were growth over 304 stainless steel using plasma enhanced chemical vapor deposition. The response surface methodology was used to develop a mathematical modeling of friction for these films, using the experimental results, in order to identify parameters that control friction and construct tribological maps according to the CD average sizes. The presence of bigger CD particles (250 and 500 nm) increased the film roughness. Films with CD particles of 4 nm presented the most homogeneous friction map, with minor variation in friction coefficient with the increase/decrease of load and sliding speed even when the CD concentration increase. This result suggests that in CD-DLC films containing CD particles of 4 nm average size, the nanoparticles are better incorporated in DLC structure due to its average size (4 nm) that is near than DLC grain size and could occupy the nanospaces between DLC grains.     

DLC nano-dot surfaces for tribological applications in MEMS devices

With the invention of miniaturized devices like micro-electro-mechanical systems (MEMS), tribological studies at micro/nano-scale have gained importance. These studies are directed towards understanding the interactions between surfaces at micro/nano-scales, under relative motion. In MEMS devices, the critical forces, namely adhesion and friction restrict the smooth operation of the elements that are in relative motion. These miniaturized devices are traditionally made from silicon (Si), whose tribological properties are not good. In this paper, we present a short investigation of nano- and micro-tribological properties of diamond-like carbon (DLC) nano-dot surfaces. The investigation was undertaken to evaluate the potential of these surfaces for their possible application to the miniaturized devices. The tribological evaluation of the DLC nano-dot surfaces was done in comparison with bare Si (1 0 0) surfaces and DLC coated silicon surfaces. A commercial atomic force microscope (AFM) was used to measure adhesion and friction properties of the test materials at the nano-scale, whereas a custom-built micro-tribotester was used to measure their micro-friction property. Results showed that the DLC nano-dot surfaces exhibited superior tribological properties with the lowest values of adhesion force, and friction force both at the nano- and micro-scales, when compared to the bare Si (1 0 0) surfaces and DLC coated silicon surfaces. In addition, the DLC nano-dot surfaces showed no observable wear at the micro-scale, unlike the other two test materials. The superior tribological performance of the DLC nano-dot surfaces is attributed to their hydrophobic nature and the reduced area of contact projected by them.     

Nanotribology of Mo–Se–C films

Transition metal dichalcogenides with a layered structure are well known for their self-lubricating properties, particularly in a vacuum or dry atmosphere. The macrotribological properties of these films have been studied extensively. However, the tribological behaviour of these films in the nanonewton load range has hardly been reported. Study of tribological properties with load in the nanonewton range is required for applications related to microelectromechanical systems or nanoelectromechanical systems. In view of the above, the hardness, surface force, friction force, etc. of Mo–Se–C films were investigated at an applied load in the nanonewton range using a nanoindenter and atomic force microscopy. The effect of carbon content, applied load and scanning speed on the friction coefficient was determined. Data pertaining to topography, lateral force and pull-off force of various surfaces are illustrated. The observed nanotribological behaviour of these films is analysed in the light of their nanohardness. The results indicate that the friction force of all the films is very low and in general dependent on surface force. However, a film having the highest carbon content exhibits the maximum friction force. With increasing carbon content of the films tested, the hardness increases and wear decreases. The above results pertain to investigations under ambient conditions.     

Tribological properties of chemically bonded polyimide films on silicon with polyglycidyl methacrylate brush as adhesive layer

Polyimide thin films, which possess good stability and film uniformity, are successfully fabricated on single crystal silicon wafers coated with a thin polymer brush by suface-initiated polymerization (SIP) as an adhesive layer. The growth kinetic of polyglycidyl methacrylate (PGMA) brush was studied by the means of ellipsometry. The nano-scale morphology and chemical composition of PGMA brush and polyimide film were studied with atomic force microscopy (AFM), Fourier transform infrared spectrum (FT-IR), and X-ray photoelectron spectroscopy (XPS). The tribological behaviors of the thin films sliding against AISI-52100 steel ball were examined on a static-dynamic friction precision measurement apparatus and UMT-2MT tribometer. The worn surface of the polyimide thin films was investigated with scanning electron microscopy (SEM). The results indicated that the chemically bonded polyimide films exhibited better friction reduction and antiwear behavior compared to the polymide films on bare silicon surface. At a load of 0.5 N and sliding speed of 20 mm s⁻¹, the durability life of the polyimide thin films is over 25,000 sliding cycles and the friction coefficient is about 0.08.