管状构件内表面真空镀膜方法研究进展

综述了国内外真空镀膜方法,包括化学气相沉积与物理气相沉积方法对管状构件内表面镀膜的研究进展,介绍了热化学气相沉积及各种等离子体(包括直流、射频及电子自旋共振等离子体)增强化学气相沉积方法在管状构件内表面镀膜方面的应用,分析了这种方法的优缺点;重点阐述了溅射镀膜方法 (包括直流二极(或三极)溅射、磁控溅射及离子束(或激光束)溅射)及电弧离子镀技术在管状构件内表面镀膜时对薄膜种类、沉积速率、薄膜厚度轴向均匀性、膜/基结合力等方面的特点。最后对管状构件内表面各种真空镀膜方法进行了分析对比,指出了存在的问题及今后的发展方向。     

热处理对两种铜膜结合强度的影响

采用PVD和CVD技术制备Cu/TiN/PI试样，研究表明，TiN薄膜可以有效地阻挡Cu向PI基板内部扩散，CVD工艺制备的Cu膜内部残余应力很小，Cu膜有相对高的结合强度；而PVD制备的Cu膜，在有TiN阻挡层存在的情况下，Cu膜内存在拉应力，拉应力降低了Cu膜结合强度，300℃退火可以消除膜内残余应力，结合强度提高。     

无黏结相PCD和PCBN材料研究进展

无黏结相PCD和PCBN具有良好的高温性能,特别是拥有纳米晶粒或纳米结构的PCD和PCBN的性能甚至高于单晶体的性能。对无黏结相聚晶立方氮化硼（PCBN）和聚晶金刚石（PCD）材料的合成方法、烧结机理及其性能进行了详细概述。在高于7 GPa和1800℃下,能烧结出致密的无黏结相PCD和PCBN材料,但不同原材料粉末和微量触媒或掺杂会对超高压高温（HPHT）烧结条件和机理产生较大的影响。基于HPHT方法的制备条件较苛刻,PVD和CVD是比较有前途的制备PCD的方法,但用于制备PCBN还需要解决许多技术问题。      

金属陶瓷及硬质合金表面CVD/PVD涂层的摩擦与切削性能

为研究涂层沉积方式对金属陶瓷和硬质合金性能的影响,采用粉末冶金技术制备了Ti(C,N)基金属陶瓷和YT15硬质合金,在基体表面先后采用CVD和PVD制备涂层。采用SEM、EDS等手段对涂层的微观组织和元素含量进行分析,并对涂层试样进行划痕、摩擦因数、切削性能检测。结果表明,通过复合CVD+PVD工艺,CVD涂层和PVD涂层结合良好。不论是金属陶瓷还是硬质合金,CVD涂层的膜基结合力和摩擦因数均为最大,PVD涂层最小,复合CVD+PVD涂层介于两者之间。对于金属陶瓷和硬质合金而言,复合CVD+PVD涂层的切削性能最好,CVD涂层最差,PVD涂层介于两者之间。切削过程中的磨损机理主要是氧化磨损和磨粒磨损。     

FeAl/Al_2O_3复合阻氚涂层制备技术的研究进展

FeAl/Al_2O_3复合膜层是聚变堆氚增殖包层及辅助涉氚系统结构材料首选的阻氚涂层。其制备过程通常需要铝化和氧化2个步骤,铝化是Al原子与基体Fe原子通过相互扩散在基体表面形成铁铝固溶体(Fe,Al)或Fe-Al金属间化合物过渡层;氧化是使铝化涂层表面选择性氧化形成Al_2O_3膜。该阻氚涂层的制备可采用物理气相沉积(PVD)、化学气相沉积(CVD)、热浸铝化(HDA)、包埋渗铝(PC)、等离子体喷涂(PS)和电化学沉积(ECD)等技术。相对而言,CVD、HDA和PC等3种技术有较好的应用前景,有望成为聚变堆中FeAl/Al_2O_3阻氚涂层工程化制备的候选技术而ECD技术因其制备过程容易控制、涂层性能稳定、可涂镀复杂结构件等特点在FeAl/Al_2O_3阻氚涂层制备方面颇具吸引力。     

Experimental design in the deposition of BN interface coatings on SiC fibers by chemical vapor deposition

Boron Nitride (BN) coatings deposited by chemical vapor deposition (CVD) have been increasingly used as an interface material for SiC/SiC composites. In this work, the CVD of BN was investigated using a statistical design of experiments (DOE) approach. In order to determine the most significant parameters for the process a two-level screening design (Plackett-Burman) was employed. The deposition pressure, gas mixture dilution factor, deposition time, and the reaction gas flow ratios were found to be the most significant factors that influenced coating thickness. To optimize the deposition process, a three-level surface response design (Box-Behnken) was used with the aim of producing a predictive mathematical model of the process. The generated response surface modeling (RSM) showed that deposition time had the greatest effect on coating thickness while, temperature-time and temperature-NH₃/BCl₃ interactions may be large at low/high NH₃/BCl₃ ratios and high deposition time, respectively. Tensile strength was strongly influenced by the deposition temperature and deposition time. The response model showed the dependence of tensile strength on coating thickness, NH₃/BCl₃ gas flow ratios and time. The model interaction plots suggested a dependence of temperature-gas flow ratio on tensile strengths of BN coated SiC fibers.     

TiSiO非晶结构光学薄膜的性能调控机理研究进展

TiSiO复合薄膜的制备方法主要包括溶胶-凝胶、物理气相沉积和化学气相沉积等,针对不同制备工艺条件下SiO2改性TiO2的微观结构与光学参量的调控机理的研究,仍处于探索阶段。综述了近年来国内外在不同工艺条件下沉积的TiSiO薄膜的结构和光学性质,从溶胶体系和热处理工艺两方面,对溶胶-凝胶工艺制备的TiSiO薄膜展开论述,分别归纳了溶胶体系和热处理工艺调控TiSiO薄膜的结构和光学性质的一般规律;从溅射工艺和蒸发工艺两方面对物理气相沉积工艺制备的TiSiO薄膜展开论述,分别阐述了在溅射工艺和蒸发工艺过程中,调控TiSiO薄膜的结构和光学性质的一般规律;从低（常）压化学气相沉积和等离子增强化学气相沉积等方面,对化学气相沉积工艺制备的TiSiO薄膜展开论述,分别阐述了在不同化学气相沉积技术中,通过调节一些重要参数调控薄膜结构和性能的一般规律。总结了不同工艺制备并调控TiSiO薄膜的一般规律的内在联系,并指出了这类薄膜制备工艺存在的问题和后续的研究方向。     

高能束在气相沉积超硬薄膜材料中的应用

在新型薄膜材料的制备中,利用高能量密度的激光束、离子束等作为热源,辅助和诱导气相反应制备薄膜材料,克服了普通化学气相沉积和物理气相沉积超硬薄膜材料性能上的不足,显著地提高了薄膜的沉积效果.     

工作气压对Y掺杂HfO2结构及电学性能的影响

目的 基于Y掺杂高纯铪靶和钛靶的反应磁控溅射方法,在Si(100)基底上沉积掺杂Y氧化铪薄膜,以及TiN/X-HfO2/TiN三层异质结构,探究Y掺杂对氧化铪基异质结构铁电性的影响。方法 针对反应磁控溅射制备的Y掺杂HfO2薄膜和异质结构,分别采用白光干涉仪、掠入射X射线衍射(GIXRD)、X 光电子能谱仪(XPS)和铁电分析仪,对薄膜的沉积速率、退火后薄膜的晶体结构、掺杂元素组分及含量,以及HfO2基异质结薄膜P-E电滞回线和I-V曲线进行测量。结果 在相同工艺条件下,薄膜的沉积速率随着工作气压的增大呈先增大后减小的趋势,在工作气压为1.1 Pa时沉积速率达到最高值。XRD结果表明,薄膜经过退火后存在正交相(o相)和单斜相(m相)。当工作气压为0.7 Pa时,所制备HYO薄膜在28°~30°内代表o(111)相的衍射峰最强,具有最佳的铁电性。随着工作气压的增大,代表m(111)相的衍射峰强度逐渐下降。采用XPS分析了薄膜中各元素的化学状态和含量,在工作气压为0.7 Pa时,Y的掺杂浓度(物质的量分数)为5.6%,铁电分析结果表明,在工作气压从0.7 Pa增至1.3 Pa的过程中,Y掺杂的HfO2基异质结的电滞回线逐渐收缩。在工作气压为0.7 Pa时,剩余极化强度Pr的最大值为14.11 µC/cm²,矫顽场Ec约为1 MV/cm。结论 利用Y掺杂高纯铪靶反应磁控溅射制备的掺杂铁电薄膜,在工作气压0.7 Pa下得到的薄膜经过700 ℃退火后具备良好的铁电性能。     

电弧离子镀法制备高硬度Cr-Si-C-N薄膜

采用电弧离子反应沉积技术在SCM415渗碳淬火钢基片上沉积了Cr-Si-C-N薄膜,三甲基硅烷(TMS)反应气体作为Si和C掺杂源,通过改变TMS流量实现了薄膜中si和C含量的调节.利用XPS,XRD,HRTEM和显微硬度计研究了Cr-Si-C-N薄膜的化学状态、显微组织和显微硬度.Cr-Si-C-N薄膜中的Si和C含量随TMS流量的增加而单调增加.在TMS流鼍小于:90 mL/min时,薄膜中Si和C含量较少,薄膜由Cr(C,N)纳米晶与Si_3N_4非品(nc-Cr(C,N)/a-Si_3N_4)组成,薄膜硬度随流量的增加而单调增大,最大至4500 HK.硬度的增加源于固溶强化及薄膜中纳米晶/非晶复合结构的形成;当TMS流量大于90 mL/min时,薄膜中Si和C含量较多,多余的C以游离态形式存在,且随TMS流量的增加而增多,薄膜硬度下降.     

High temperature processing of poly-SiC substrates from the vapor phase for wafer-bonding

The transfer by wafer-bonding of single-crystalline SiC thin films to a polycrystalline SiC substrate to obtain a “quasi-wafer” requires high quality polycrystalline substrates with controlled bulk properties (thermal conductivity, electrical resistivity) as well as with very low surface roughness (RMS < 5 nm) and bowing (< 10 μm). Currently, available polycrystalline SiC wafers are processed by sintering or by Chemical Vapor Deposition (CVD). Sintered ceramic wafers are very heterogeneous (mixture of 3C, 6H, 4H and silicon), while CVD ones are of better quality (homogeneous and textured 3C). The aim of this paper is to investigate the fabrication and the properties (bulk and surface) of SiC substrates with large (0.1 to a few mm) grains. To meet these requirements, two high temperature processes (around 2000 °C) for single crystal growth were used: Physical Vapor Transport (PVT) and the recently developed CVD Feed Physical Vapor Transport (CF-PVT). Structural investigations performed on large grain wafers sliced and polished from the grown ingots showed an important influence of the initial seed on the grain size, polytype and crystallographic texture. Chemical and Mechanical Polishing (CMP) of such structures was studied and optimized to obtain low surface roughness. The intra-grain roughness is very low (RMS < 0.5 nm) but a few nanometer of height steps were observed between grains. The relations between bulk properties, surface functionalization and process conditions are discussed. This first seeding step with commercial substrates is necessary for the creation of original substrates which can be used for the fabrication of new substrates.     

A kinetic investigation of CVD mullite coatings on Si-based ceramics

Chemically vapor deposited (CVD) mullite coatings were deposited on SiC substrates using the AlCl₃,SiCl₄,CO₂,H₂ system in a hot-walled vertical type reactor. An empirical kinetic model was developed indicating that an intermediate gaseous reaction was kinetically significant to the growth rate of mullite on SiC. The kinetically limiting equation was defined between a temperature range of 673–1327 K and 30–400 mbar where temperature was defined as a function of reactor position. The growth rate and crystal structure of mullite were dependent upon temperature, pressure, reactant concentration, and reactant ratios.     

金属钨箔膜的制备研究进展

具有体密度的高表面质量金属钨薄膜对材料高压状态方程研究具有十分重要的意义.综述了钨箔膜制备的几种方法,包括化学气相沉积、物理气相沉积、机械轧制、机械研磨抛光、化学抛光和电解抛光.综合比较后认为,采用电解抛光法可以基本满足状态方程靶用钨箔膜的需要.电解抛光可以制备表面质量比较高,厚度最小可达几微米的金属箔材,密度与原料相同,而且不会产生内应力、表面硬化、表面沾污问题,是制备低表面粗糙度、具有块材组织结构和密度材料的一种重要手段.     

C芯SiC纤维制备技术研究

在自行设计制造的直流电阻加热CVD装置上制备出C芯SiC纤维,C芯SiC比W芯具有更高的力学性能,更好的界面相容性,更低的密度,成为制备SiC/Ti基复合材料的最佳增强体。研究CH3SiHCl2-CH3SiCl3-H2-Ar体系中在C芯表面化学气相沉积SiC涂层工艺,考察沉积温度,[H2]/[silane],气流量,Ar气流量对化学气相沉积SiC涂层的结构、性能的影响。并对涂层表面形貌及结构成分进行SEM,XRD,raman,AES分析。结果表明:在温度1200℃,[H2]/[silane]=1.4,气体流量4.89L/min,稀释气体0.2L/min时,纤维拉伸强度最好为3392MPa。其中纤维的性能对沉积温度,[H2]/[silane]最敏感。     

原位生长碳纳米管及其在SiC_f/SiC复合材料中的应用

采用碳纳米管改善纤维与基体间的界面结合,同时利用碳纳米管自身的优异性能对碳化硅纤维增强碳化硅复合材料(SiCf/SiC)进行二次增强。通过化学气相沉积工艺(CVD)在SiC纤维编织件内原位生长碳纳米管,优化碳纳米管原位生长过程中的碳源流量、反应温度和反应时间等工艺参数,对碳纳米管的原位生长工艺及机理进行系统分析,并结合先驱体浸渍裂解工艺(PIP)制备CNTs-SiCf/SiC复合材料,探讨原位生长碳纳米管的引入对复合材料力学性能的影响。结果表明,优化后的工艺参数如下:反应温度750℃,C2H2、H2和N2流量比1/1/3,C2H2流量100~150 mL/min,反应时间60 min;碳纳米管的引入使SiCf/SiC复合材料的弯曲强度、弯曲模量和断裂韧性分别提高了16.3%、90.4%和106.3%。     

Effects of Growth Parameters on the Morphology of CNTs/Cu Composite Powder Prepared Using Cr/Cu Catalyst by Chemical Vapor Deposition

采用化学共沉淀法制备了Cr/Cu复合粉体催化剂,并用化学气象沉淀法（CVD）原位合成CNTs/Cu复合粉末。利用SEM, TEM和Raman光谱分别对其微观形貌和结构进行表征。结果表明：采用化学气相沉淀法,使用10 wt%Cr/Cu 的催化剂,在混合气体(Ar/H2/C2H4) 流量2450/300 mL/min下,于1073 K 温度生长30 min,可以得到优质、结晶良好的 CNTs/Cu 复合粉末     

材料表面技术的研究及双辉技术在防腐蚀中的应用

文章简要介绍了化学气相沉积（CVD）、物理气相沉积（PVD）、高能束表面改性及其它表面处理技术的新进展,讨论了利用双辉离子渗技术处理后碳钢对酸液的耐腐蚀性能.经双辉技术处理后的碳钢试样在稀硫酸和富液中的耐腐蚀性能显著提高.     

Chemical Vapor Deposition and Atomic Layer Deposition of Coatings for Mechanical Applications

Chemical vapor deposition (CVD) of films and coatings involves the chemical reaction of gases on or near a substrate surface. This deposition method can produce coatings with tightly controlled dimensions and novel structures. Furthermore, the non-line-of-sight-deposition capability of CVD facilitates the coating of complex-shaped mechanical components. Atomic layer deposition (ALD) is also a chemical gas phase thin film deposition technique, but unlike CVD, it utilizes “self-limiting” surface adsorption reactions (chemisorption) to control the thickness of deposited films. This article provides an overview of CVD and ALD, discusses some of their fundamental and practical aspects, and examines their advantages and limitations versus other vapor processing techniques such as physical vapor deposition in regard to coatings for mechanical applications. Finally, site-specific cross-sectional transmission electron microscopy inside the wear track of an ALD ZnO/ZrO₂ 8 bilayers nanolaminate coating determined the mechanisms that control the friction and wear.     

连续纤维增主基复合材料研究概况

重点了介绍了连续纤维境强钛基复合材料的３种复合方法,即箔材－纤维－箔材法、等离子喷射涂层法和物相沉积法,开发的强化纤维有ＳｉＣ纤维和Ａ１２Ｏ３单晶纤维,并介绍了它们的研究进展,最后讨论了一些复合材料的性能循呼复合材料的损伤评价技术。     

Low-pressure synthesis of polycrystalline diamond abrasive

Polycrystalline diamond abrasives are used extensively for grinding of cemented tungsten carbide. Although these diamond crystals are somewhat weaker than the well formed cubo-octahedral crystals, they are ideal for grinding cemented carbide without causing surface integrity problems (metallurgical damage and microcraking due to thermal and mechanical stresses). Polycrystalline diamond of this type is currently produced by the high-pressure—high-temperature (HP-HT) technique. In this paper, we report an alternative technique for the production of polycrystalline diamond abrasive, namely combustion synthesis, using a simple oxy-acetylene torch. Although the growth rates by this technique are currently two orders of magnitude lower than the HP-HT technique, in view of the simplicity of this technique, the low cost of equipment as well as the lower running and maintenance costs (compared to the HP-HT presses, dies, power, etc.) activated chemical vapor deposition (CVD) diamond synthesis has potential for becoming an alternative approach to the growth of diamond crystals for abrasive applications. The situation will be more favorable with further advances in the low-pressure, activated CVD processes, which are still in their initial stages of development (similar to the HP-HT situation in the late 1950s), while the HP-HT process is more or less a matured technology.