PECVD法硅基氮化硅薄膜的制备及其耐磨性研究

以N(111) 型的单晶硅片为基体,运用PECVD-2D等离子体化学气相淀积台在单晶硅片表面沉积氮化硅薄膜,通过薄膜颜色与厚度间的关系探讨了制备工艺参数对薄膜厚度的影响,用原位纳米力学测试系统对氮化硅薄膜的纳米硬度进行测定,在UMT-2型摩擦试验机上对不同制备工艺的硅基氮化硅薄膜进行耐磨寿命试验.结果表明:随着沉积温度的升高,薄膜厚度逐渐递减,SiH4和N2流量比越大,薄膜厚度越大;温度越高,薄膜硬度越大,耐磨寿命越长;随着SiH4和N2流量比的增加,薄膜硬度和耐磨寿命均先增加后减小.     

PECVD氮化硅薄膜性质及工艺研究

为了制备高质量氮化硅薄膜,采用等离子体增强化学气相沉积(PECVD)进行氮化硅的气相沉积,讨论了工艺参数对薄膜性能的影响,验证设备工艺均匀性和批次间一致性。通过高低频交替生长低应力氮化硅薄膜,并检测薄膜应力,对工艺进行了优化,探索最佳的高低频切换时间。研究了PECVD氮化硅薄膜折射率、致密性、表面形貌等性质,制备出了致密的氮化硅薄膜。研究结果表明,PECVD氮化硅具有厚度偏差小、折射率稳定等特点,为其在光学等领域的应用打下了基础。     

Lubrication of Silicon Nitride and Silicon Carbide by Water: Running in,Wear and Operation of Sliding Bearings

The purpose of this work was to establish the conditions for the operation and break-in of water-lubricated ceramic bearings. The experiments consisted of sliding 1/4 silicon nitride or—carbide balls against pre-polished disks of the same material in water until tribochemical wear generates smooth conformal surfaces that allow hydrodynamic lubrication (<0.002) by very thin water films. This running in was performed at various sliding speeds (0.01-4m/s) and loads (0.5-20N). The minimum sliding speed for low friction were 0.04m/s for silicon nitride and 0.5m/s for silicon carbide, much lower than for conventional bearings. The load carrying pressures were 60-80MPa, which is higher than the usually pressures of thrust bearings. The hydrodynamic fluid film thickness was estimated with a standard integration of Reynolds' equations modified for circular geometry, it was to be 5-15nm for silicon nitride, 25nm for silicon carbide. Operation over long distances (80km) allowed us to measure the wear rate during hydrodynamic lubrication; this was found to be <2×10^–11mm³/nm, a rate acceptable for industrial application. A novel method completed during this work allows the determination of the wear rate during run-in. It varies with sliding velocity for silicon nitride, from 1 to 6×10^–5mm³/nm; it is constant at 4×10^–6mm³/nm for silicon carbide.     

一种电容式硅微机械麦克风的设计与制造

给出了一种电容式硅微机械麦克风的设计和制造方法。该微机械麦克风在单一硅片上制作,麦克风的两个电极由1个3层复合敏感膜和1个带有通气孔的金属铜底板构成,敏感膜与底板之间采用牺牲层技术形成空气问隙。测试结果表明,该硅微机械麦克风适合在工业界推广应用。     

PECVD制备光学氮化硅薄膜均匀性分析研究

采用等离子体增强化学气相沉积(PECVD)技术制备的光学薄膜,其均匀性受到多种工艺参数的影响,在这些参数中,一类是沉积过程的工艺参数;另一类则是设备结构参数,设备结构参数决定着反应腔室内气流分布、以及电场分布等。通过改变沉积过程的工艺参数和一组正交试验,分析各个工艺参数对均匀性的影响,从而改善氮化硅薄膜均匀性。     

A Device for Sublimation Molecular-Beam Deposition of Silicon Films

A device for sublimation molecular-beam deposition of P-doped silicon films on standard silicon wafers with diameters of up to 76 mm is described. Uniform deposition was performed through asymmetric arrangement of the sublimation source relative to the wafer, which was rotated about its axis.     

Silicon Nitride Rolling Bearings for Extreme Operating Conditions

The high hardness and excellent high-temperature performance of ceramics are attractive for critical rolling-bearing applications, such as in high-thermal-efficiency engines. In addition, the lower density of ceramics permits lower centrifugal loads, less skidding at high speeds, and, consequently, results in longer bearing component life than conventional bearing steels or alternative super-alloys or cermets. Silicon nitride has the lowest friction and elastic modulus of the available ceramics, which reduce bearing contact stresses. This paper reviews the merits and demerits of silicon nitride as a bearing material, its processing, and different mechanisms for solid-lubricant replenishment in severe environments. Test data and application design guidelines accumulated to dale are also provided.     

脉冲激光沉积薄膜的残余应力测量

为了测量脉冲激光沉积法制备的小面积薄膜的残余应力,并解决Stoney公式在特定情况下误差较大的问题,本文提出了一种基于悬臂梁结构和数值计算的薄膜残余应力测量方法。该方法以初始曲率为零的原子力显微镜探针作为衬底梁,在衬底梁上使用脉冲激光沉积方法沉积被测薄膜,并记录衬底梁在薄膜沉积前后的翘曲形貌变化,再结合薄膜厚度、衬底梁几何尺寸、所涉及材料的杨氏模量与泊松比等其他参数,借助数值计算对实验数据进行分析,得出被测薄膜的残余应力。使用该方法测出:基于脉冲激光沉积法在高温环境下制备的二氧化钒薄膜的残余应力为-340 MPa,与文献报道的结果相符。本文提出的基于悬臂梁结构和数值计算的薄膜残余应力测量方法具有适用范围广、准确度好、实验成本低的优点。     

SiH2CL2-NH3-N2体系LPCVD Si3N4薄膜因素分析

以二氯甲硅烷和氨气分别作为低压化学气相淀积(LPCVD)氮化硅(Si3N4)薄膜的硅源和氨源,以高纯氮气为载气,在热壁型管式反应炉中反应生成Si3N4薄膜.考察了工作压力、反应温度、气体原料组成等因素对Si3N4薄膜淀积速率的影响.结果表明Si3N4薄膜的生长速率随着工作压力的增大单调增大,随着原料气中氨气和二氯甲硅烷的流量之比的增大单调减小.随着反应温度的升高,淀积速率逐渐增加,在840 ℃附近达到最大,随后迅速降低.在适当的工艺条件下,制备的Si3N4薄膜均匀、平整.较低的薄膜淀积速率有助于提高薄膜的均匀性,降低薄膜的表面粗糙度.     

氮化硅粉体水基悬浮液电动特性的研究

通过测量氮化硅粉体在水溶液中的Zeta电位和颗粒大小,研究了不同条件下氮化硅水基悬浮液的电动特性。结果表明：氮化硅粉体的等电点在pH=4．2处,溶液的pH值以及引入的聚电解质均会使氮化硅颗粒表面的荷电状态发生变化,进而导致粉体在水溶液中的分散状况发生改变。在碱性条件下,添加适量的阴离子聚电解质NH4PAA有利于氮化硅水基悬浮液的稳定分散,而过量的NH4PAA会导致颗粒的重新团聚。     

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.     

Tribological and mechanical properties of carbon nitride thin coating prepared by ion-beam-assisted deposition

Carbon nitride thin films may become good competitors for diamond-like carbon, due to their high hardness, high wear resistance, and low friction coefficient. At present, there are only a few studies of the effect of CN _x coating hardness and internal stress on its tribological properties, such as coating life and frictional behaviour. This work deals with tribological and mechanical properties of a carbon nitride coating prepared by ion-beam-assisted deposition (IBAD). Friction coefficients in the range of 0.10–0.12 were observed for the best CN _x coatings sliding against silicon nitride under ambient conditions. A nonlinear correlation between coating life and its internal stress and hardness was found.     

Silicon Nitride Boundary Lubrication: Lubrication Mechanism of Alcohols

This paper describes the lubrication mechanism of alcohols with silicon nitride under boundary lubrication conditions. Dynamic wear tests and static chemical reaction studies were conducted to study the chemical interaction between alcohols and silicon nitride. Direct evidence of chemical reactions occurring between alcohols and silicon nitride was collected. Gel-permeation-chromatography-graphite-furnace-atomic-absorption (GPC-GFAA) analysis detected the presence of high molecular weight (HMW), silicon-containing, metallo-organic compounds in the wearing contact. Secondary ion mass spectrometry (SIMS) analysis of the reaction products from wear tests revealed the formation of silicon alkoxides. These alkoxides subsequently reacted to form HMW products which had been independently verified as capable of lubricating silicon nitride surfaces. A two-ball collision test was used to verify the lubricating quality of the film generated from the wear test. A lubrication mechanism is proposed in which alcohols adsorb and react with the oxide/hydroxide layer of Si₃N₄ to produce a bonded surface silicon alkoxide. Subsequent tribochemical reactions prompted by the surface disruption from the wearing contact cause the formation of free silicon alkoxides. These species then proceed to form a variety of silicon-containing high molecular weight products that have demonstrable lubricating ability. This mechanistic understanding provides a framework of Si₃N₄ lubrication.     

离子束增强沉积薄膜的摩擦磨损行为与结构分析

采用离子束增强沉积（IBED）技术在不锈钢1Cr18Ni9Ti衬底表面生长氮化钛薄膜以及氮离子注入,进行了干滑动摩擦磨损试验与组织结构电镜分析,表明增强沉积膜较离子注入具有更高耐磨性能。     

Nano‐scratch study of molecular deposition films on silicon wafers using nano‐indentation

Experiments on molecular deposition (MD) films with and without alkyl terminal groups deposited on silicon wafers were conducted using nano‐indentation. It was found that MD films and alkyl‐terminated MD films exhibit a higher critical load and a lower coefficient of friction than the silicon substrate. The critical load increases with the number of layers, and the coefficients of friction of MD films with alkyl terminal groups are lower than those of the corresponding MD films with the same number of layers but without alkyl terminal groups.     

Evaluation of Hot Pressed Silicon Nitride as a Rolling Bearing Material

A series of tests has been conducted to evaluate the suitability of silicon nitride as a bearing material for rolling contact applications. The ability of silicon nitride to be lubricated by some conventional lubricants was found to be satisfactory. This was determined by wettability studies, lubricant film thickness and traction coefficient measurements on the optical EHD rig and friction coefficient measurements by the pin-on-disk method. The abrasive wear coefficient, measured on a lopping machine using 600 grit SiC abrasive, was found to be high compared to other ceramics. It was also dependent on the composition of the silicon nitride. Comparative rolling contact fatigue tests on steel and silicon nitride flat washers were conducted using steel rollers and balls. A high wear rate leading to grooving in the rolling track on silicon nitride was observed. The spalling resistance of silicon nitride was found to be higher than that of steel under the test conditions used. Surface interactions in the Si₃N₄-M50 steel contacts, detrimental to the life of the steel rolling elements, were recognized. Attempts were made to reduce the severity of these interactions and prolong the life of bearings containing ceramic elements.     

Quantitative measurement of repetitive impact damage on ground silicon nitride surfaces

Structural ceramics are finding application in automotive and truck engines. Poppet valves and valve seats, for example, require resistance to surface damage from repetitive impacts. Grinding and finishing processes can leave microcracks or residual stresses in the surfaces of ceramics which can accelerate surface-initiated degradation processes. A ball-on-inclined plane, repetitive impact testing system has been developed to study the effects of finishing method on surface durability. Tests were performed by repeatedly striking ground alumina and silicon nitride flat specimens with a silicon nitride sphere and measuring the impact damage as a function of the number of strikes. One type of alumina and three types of silicon nitride ceramics were tested. A quantitative impact damage parameter (IDP), based on mechanical stylus profiling data, was developed for use in measuring small amounts of wear. When damage did not extend beyond the depth of valleys in the machined surfaces, the IDP exhibited an excellent linear correlation with the number of impacts of silicon nitride on both silicon nitride and alumina materials. When more extensive damage occurred, a method involving digitizing the area of the contact damage from photomicrographs provided a reasonable correlation with number of impacts. These two methods are compared. Scanning electron microscopy revealed features which can affect the accuracy of impact damage measurement. Implications of the technique are discussed.     

真空电弧沉积薄膜显微硬度与工艺参数的关系

测试了各种工艺条件下真空电弧沉积 (VAD)的TiN薄膜的显微硬度 ,并研究了TiN薄膜硬度随基材、电弧电流、基片温度、氮气压力及负偏压的变化。实验结果表明 :在多数基材上 ,薄膜硬度均接近或超过 2 0GPa ,且薄膜的硬度与基材的硬度不呈比例关系 ,TiN薄膜的硬度随电流的增加有减少的趋势 ;在相当宽的温区内 ,TiN薄膜的硬度随温度上升而增大 ,而且在高温下的硬度值比低温时稳定 ,总体上 ,VAD比其它离子镀具有更宽阔的T区 ;在氮气压力为 0 .1Pa～ 1Pa的区域内 ,TiN薄膜的硬度稳定在 2 0MPa以上 ,而且适当的负偏压有利于提高TiN薄膜的硬度。     

基于MEMS技术硅微悬臂梁制作工艺研究

针对非制冷红外热成像中的双材料硅微悬臂梁阵列的结构要求,在MEMS常见加工工艺的基础上,提出了单个硅微悬臂梁的制作工艺路线。工艺中使用高浓度HF溶液释放牺牲层磷硅玻璃（PSG）。探讨了双层材料氮化硅和铝之间的断裂及氮化硅和硅基底之间的粘连问题,对工艺中影响成品率的关键因素残余应力进行了分析。     

氮化硅陶瓷球滚动接触疲劳寿命模型

针对球与圆柱接触模型中的陶瓷球,利用WEIBULL断裂统计方法导出球疲劳失效概率与寿命之间的关系方程,在相关额定寿命与最大接触应力的数值解基础上,基于最大主拉应力,构建氮化硅陶瓷球的滚动接触疲劳寿命与接触应力的数学模型.经与不同接触应力水平下的滚动接触疲劳寿命试验结果验证,表明该拉应力一寿命模型的正确性,从而验证了氮化硅陶瓷球的滚动接触疲劳失效源于最大主拉应力,而非基于最大切应力的设想.通过与L.P切应力一寿命模型预测结果的比较,表明拉应力一寿命模型适合于陶瓷球的接触疲劳寿命预测.