低浓度氮气对MPCVD法制备金刚石膜的影响

利用微波等离子体化学气相沉积(MPCVD)法,在CH4/H2的混合反应气源中加入N2进行了金刚石膜的沉积实验,详细研究了N2浓度对金刚石膜生长的影响规律。使用扫描电子显微镜、激光拉曼光谱仪和X射线衍射仪等设备,表征了金刚石薄膜的表面形貌、相组成及晶面取向。实验结果表明:随着N2体积分数的增加(由0%增加到6%),薄膜中的非金刚石相含量逐渐增大,金刚石晶粒尺寸逐渐减小,晶面取向也由较大的晶面(111)转变成较小的晶面(100);当N2体积分数为4%时,沉积的金刚石膜表面为"菜花"状结构;低体积分数(2%)的N2有利于获得高度取向(100)的金刚石膜。     

不同高浓度气体对金刚石薄膜制备的影响

采用微波等离子体化学气相沉积(MPCVD)法,分别制备了CH4/H2体系、CH4/H2/N2体系以及CH4/H2/Ar体系金刚石薄膜。主要采用了扫描电子显微镜(SEM)、激光拉曼光谱(Raman)和X射线衍射光谱(XRD)等方法对不同体系中制备的金刚石薄膜的晶粒尺寸及其品质进行了分析,研究了不同高浓度气体对金刚石薄膜的影响。结果显示:利用高浓度的甲烷可以在很大程度上细化晶粒,制备出纳米晶金刚石薄膜,但是薄膜的非晶相较多,品质下降;加入70%N2,薄膜中的金刚石晶粒生长速度较慢,但可制备出均匀的纳米晶金刚石薄膜;70%的Ar气氛中,金刚石晶粒生长较快,制得的薄膜中的金刚石晶粒是微米级别的。     

纳米金刚石薄膜制备的现状与展望

与微米金刚石薄膜不同，纳米金刚石薄膜晶粒度小，表面平滑。从发展水平来看，目前国内外纳米金刚石薄膜的研究，还处于基础性研究阶段，纳米金刚石薄膜的应用刚刚起步，距产业化还有较大距离。但是，由于纳米金刚石薄膜具有众多的优异性能，正因为如此，可望在众多的高技术领域中得到广泛应用。     

金刚石薄膜的合成和应用

对金刚石薄膜的合成，性质和应用进行了综述，并讨论了这一领域中存在的主要问题及研究趋势。     

甲烷浓度对金刚石薄膜织构的影响

采用热丝化学气相沉积法,以甲烷和氢气为反应气体,在硬质合金YG6基体上沉积了金刚石薄膜。研究了不同的甲烷浓度对金刚石织构变化趋势的影响。分别采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)对金刚石膜的表面形貌、织构形成进行了分析。结果表明:当基体温度为760℃,沉积气压为4×103Pa,甲烷浓度从1%到5%,都形成了(110)织构。但是,当甲烷浓度为3.3%时,有(100)织构。     

低功率MPCVD制备金刚石薄膜

通过微波等离子体化学气相沉积(MPCVD)法,以CH4/H2为气源,合成高质量金刚石薄膜,在150 W低微波功率下,从衬底预处理方法、沉积气压、流量比等方面对制备高质量金刚石薄膜的工艺参数进行研究.结果表明:高流量比不利于金刚石颗粒的粒径控制,二次形核的存在可以获得近纳米级颗粒尺寸的金刚石薄膜;较大的沉积气压有利于制备...     

热丝法气相沉积金刚石薄膜的影响因素

由于热丝法气相沉积金刚石薄膜成膜质量好、设备简单、成本低而得到广泛应用。本文探求了工具上应用最广泛的硬质合金上利用热丝法沉积金刚石薄膜的原理,并着重讨论了在该系统中影响金刚石薄膜质量的几个因素：预处理技术、碳源浓度、温度和气压,在金刚石的形核时期和生长时期这些因素的作用是不同的,同时这些因素又相互影响。根据影响因素制定出了最优的工艺参数,最后在硬质合金上得到了均匀而致密的金刚石薄膜,经XRD分析,由（111)和(220)晶面组成,主要是(111)面,晶粒尺寸平均为113．5nm,这些探索为金刚石沉积技术在工具上的大规模应用打下了基础。     

Time-modulated chemical vapor deposition of diamond films

This article investigates the role of substrate temperature in the deposition of diamond films using a newly developed time-modulated chemical vapor deposition (TMCVD) process. TMCVD was used to deposit polycrystalline diamond coatings onto silicon substrates using hot-filament chemical vapor deposition system. In this investigation, the effect of (a) substrate temperature and (b) methane (CH₄) content in the reactor on diamond film deposition was studied. The distinctive feature of the TMCVD process is that it time-modulates CH₄ flow into the reactor during the complete growth process. It was noted that the substrate temperature fluctuated during the CH₄ modulations, and this significantly affected some key properties of the deposited films. Two sets of samples have been prepared, in each of which there was one sample that was prepared while the substrate temperature fluctuated and the other sample, which was deposited while maintaining the substrate temperature, was fixed. To keep the substrate temperature constant, the filament power was varied accordingly. In this article, the findings are discussed in terms of the CH₄ content in the reactor and the substrate temperature. It was found that secondary nucleation occurred during the high timed CH₄ modulations. The as-deposited films were characterized for morphology, diamond-C phase purity, hardness, and surface roughness using scanning electron microscopy, Raman spectroscopy, Vickers hardness testing, and surface profilometry, respectively.     

硅掺杂CVD金刚石薄膜

研究硅掺杂对CVD金刚石薄膜形貌、结构特性和成分的影响。通过向丙酮中加入正硅酸乙酯作为反应气体,在硅基底上沉积硅掺杂CVD金刚石薄膜。金刚石薄膜的表面形貌和显微组织由场发射电镜表征。金刚石薄膜的成分通过拉曼光谱和X射线衍射（XRD）进行研究。薄膜的表面粗糙度由表面轮廓仪评估。结果表明,硅掺杂会降低晶粒尺寸,促进晶粒细化并抑制三角锥形形貌。XRD研究表明,（111）朝向的晶面显著减少。拉曼光谱研究表明,硅掺杂会促进薄膜中硅碳键的形成以及非金刚石相的增多。在硅碳浓度比为1％时,沉积得到光滑的细晶粒金刚石薄膜。     

直流等离子体-热丝化学气相沉积金刚石薄膜的研究

通过在传统热丝化学气相沉积装置中引入直流等离子体,设计了直流等离子体-热丝化学气相沉积金刚石薄膜的设备,设备中既包括相互独立的灯丝电压和施加的偏压。通过调节偏压可以控制所形成的等离子体的偏流。在这一改进的系统中研究了金刚石薄膜形核和生长过程,利用扫描电子显微镜（SEM）、X射线衍射（XRD）分析了金刚石的样品,结果表明,施加偏压不仅能大大促进金刚石的形核密度（10^10cm^-2）、提高金刚石薄膜的生长速率,金刚石薄膜的取向也随机取向变为（111）定向生长。     

Plasma-enhanced chemical vapor deposition of polyperinaphthalene thin films

Plasma-enhanced chemical vapor deposition (PECVD) has been used to grow corrosion-resistive, semiconducting thin films of the graphite-like polymer polyperinaphthalene (PPN) from 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA). Unlike thermal chemical vapor deposition of PPN from PTCDA, where thin film growth is catalyzed by a transition metal substrate, PPN films have been grown by PECVD for the first time on non-catalytic substrates: indium tin oxide (ITO)-coated glass, aluminum and silicon. Films with the same morphology and molecular characteristics have also been grown on steel substrates, where iron functions as a growth catalyst. Potentiodynamic corrosion measurements in pH 5 water show that PPN films on steel provide an effective corrosion protection layer.     

硬质合金基体金刚石薄膜摩擦学性能研究的进展

硬质合金基体表面沉积金刚石薄膜可以提高其硬度和耐磨性,延长其使用寿命,有效保护和节约钨、钴等稀有金属。作为一种多晶膜,金刚石薄膜的摩擦系数直接影响了其在摩擦学领域的应用。对近年来硬质合金基体表面CVD金刚石薄膜的摩擦磨损性能的研究状况进行了阐述,分析了CVD金刚石薄膜在摩擦实验过程中的摩擦磨损机制,并对金刚石薄膜在摩擦学领域中的应用研究进行了展望。     

Hot-filament chemical vapor deposition of polycrystalline diamond coatings to interlayered steel

Zr-based nitride and carbide coatings have been deposited on high-speed steel by the cathodic arc method. Hot-filament chemical vapor deposition (CVD) has been used to deposit diamond films onto a treated steel surface. The films deposited by CVD were characterized using scanning electron microscopy, x-ray diffraction, and Raman spectroscopy to determine the surface morphology, roughness, crystal structure, and bonding characteristics. This paper was presented at the fourth International Surface Engineering Congress and Exposition held August 1–3, 2005 in St. Paul, MN.     

沉积参数对硬质合金基体微/纳米金刚石薄膜生长的影响

基体温度、反应压力和碳源浓度等沉积参数决定热丝化学气相沉积金刚石薄膜的性能。运用正交试验方法,研究参数对硬质合金基体金刚石薄膜生长的综合作用。采用场发射扫描电镜（FE-SEM）、原子力显微镜（AFM）和拉曼（Raman）光谱检测薄膜的形貌结构、生长速率和成分。结果表明：随着基体温度的降低,金刚石形貌从锥形结构向团簇状结构转变;低反应压力有利于纳米金刚石薄膜的生成;生长速率受反应压力和碳源浓度综合作用的影响。     

在CH4-H2微波等离子体中添加H2O对大面积金刚石膜生长的研究

用自制的微波功率为5千瓦的微波等离子体（MWCVD）装置，研究了在CH4-H2反应气体中添加安全廉价的H2O代替O2金刚石膜的沉积状况，以H2／CH4／H2O作为反应气体，成功制备了厚度达到1．1毫米，面积达20平方厘米的金刚石厚膜。在沉积温度为700-900℃范围内，研究了CH4／H2=3.0％，H2O／H2=0．0-2．4％范围内金刚石膜沉积的速率，均匀性，形貌以及质量的变化规律。研究结果表明，在反应气体CH4／H2中添加适量H2O能降低金刚石膜中非金刚石碳的含量，提高金刚石膜厚度的均匀性，并对反应气体中添加H2O对CVD金刚石膜生长影响机理进行了阐述。     

Properties of chemically vapor deposited blanket tungsten films on tin glue layers prepared by chemical vapor deposition

The dependence of CVD W growth on various types of TiN layers was investigated with blanket and patterned wafers. There were no appreciable effects of the properties of TiN on the resistivity, structure, growth rate or reflectivity of CVD W in the case of blanket wafers; however, the stress of the W layer was found to be dependent upon the type of TiN glue layer adopted. W deposited on the TDMAT-TiN glue layer exhibits the lowest stress levels among the tested TiN films. TiCl₄-TiN proved to be superior to TDMAT-TiN from the viewpoint of W conformality. Although there was no appreciable effect of deposition temperature silane reduction time, contact size or shape of contact upon the W conformality on a TiCl₄-TiN layer, the W conformality on TDMAT-TiN was highly dependent on the above parameters, apparently caused by insufficiently plasma treated TiN on the side walls of contacts.     

化学气相沉积法制备铼材料的研究进展

铼具有优异的物理力学性能,作为功能材料及超高温结构材料获得广泛应用。铼材料的制备方法有多种,化学气相沉积（CVD）是其主要的制备方法之一。本文简要介绍了化学气相沉积制备铼材料的反应类型、沉积条件及沉积效果,综述了CVDRe材料的沉积动力学、组织结构特征、力学性能的研究现状和典型应用,并与粉末冶金铼进行了对比分析。最后指出了目前CVDRe材料研究亟待解决的关键问题,并对进一步研究的方向和推广应用前景进行了展望。