SiC在异质衬底生长金刚石膜的作用分析

利用扫描电子显微镜 (SEM)、Raman光谱分析了Si衬底上金刚石膜核化和生长的过程 ,并着重分析了核化过程产生的SiC的性能。利用划痕法测量了在WC衬底上沉积SiC和未沉积SiC时生长金刚石膜的粘附力 ,同时还分析了WC衬底上有和没有SiC沉积层时表面附近金刚石膜的内应力。结果表明 ,SiC层大大地增强了含碳粒子的聚集和金刚石膜与衬底之间的粘附性 ,降低了金刚石膜与衬底之间的内应力     

大面积平整金刚石薄膜的制备

用热丝CVD的方法在3英寸的硅衬底上生长均匀的金刚石薄膜。应用了在热丝上方加石黑电极,在形核阶段相对于热丝施加一直流负偏压的预处理方法,使金刚石的成核密度达到10^10-10^11/cm^2,在3英寸镜面抛光的硅衬底上制备了平整的金刚石薄膜,生长的薄膜用SEM及喇曼光谱进行了测试。实验发现电极的位置是影响金刚石薄膜均匀性的重要因素。     

SiC在异质衬底生长金刚石膜的作用分析

利用扫描电子显微镜（ＳＥＭ）、Ｒａｍａｎ光谱分析了Ｓｉ衬底上金刚石膜核化和生长的过程,并着重分析了核化过程产生的ＳｉＣ的性能。利用划痕法测量了ＷＣ衬底上沉积ＳｉＣ和未沉积ＳｉＣ时生长金刚石膜的粘附力,同时还分析了ＷＣ半底上有和没有ＳｉＣ沉积层时表面附近金刚石膜的内应力。结果表明,ＳｉＣ层大大地增强了含碳粒子的聚集和金刚石膜与衬底之间的粘附性,降低了金刚石膜与衬底之间的内应力。     

基于硅过渡层纳米金刚石膜/GaN复合膜系的制备（英文）

本文研发了一种简便有效的在GaN半导体衬底上直接生长纳米金刚石膜的方法。研究发现,直接将GaN衬底暴露于氢等离子体中5 min即发生分解,且随着温度从560℃升高至680℃,这种分解反应愈加剧烈,很难在GaN衬底上直接形成结合力良好的纳米金刚石膜。通过在GaN衬底上镀制几纳米厚的硅过渡层,在富氢金刚石生长环境下,抑制了GaN衬底的分解,同时在GaN衬底上沉积了约2μm厚的纳米金刚石膜。硅过渡层厚度是决定纳米金刚石与GaN衬底结合力的主要因素。当硅过渡层厚度为10 nm时,纳米金刚石膜与GaN衬底呈现出大于10 N的结合力,可能与硅过渡层在金刚石生长过程中向SiC过渡层转变有关。     

WC和Si衬底生长金刚石薄膜的研究

采用ＳＥＭ,Ｒａｍａｎ光谱等手段,较全面系统地研究了ＨＦＣＶＤ法在ＷＣ和Ｓｉ衬底上生长金刚石薄膜时,衬底预处理、碳源深度、热丝及衬底温度等对金刚石形核、生长的影响。并对两种衬底进行了对比与分析,最后总结出影响金刚石形核密度、形核速率、晶形结构及晶形完善性的关键因素。     

氢氧等离子体预处理对单晶金刚石刻蚀坑的研究

采用自制的微波等离子体化学气相沉积装置,在高温高压法合成的金刚石的衬底上外延生长单晶金刚石。实验分为两步,首先用氢氧等离子体在生长之前进行预处理刻蚀,然后外延生长30 h。利用金相显微镜和激光拉曼光谱来表征单晶金刚石刻蚀坑以及外延生长的单晶金刚石质量。研究结果表明,氧会优先刻蚀籽晶表面的缺陷和位错,可以通过刻蚀坑密度来判断衬底质量,且经过预处理刻蚀能消除单晶金刚石表面的缺陷。籽晶表面经刻蚀后会出现平底型和尖锥型两种倒金字塔型刻蚀坑,且晶体表面的原本缺陷或由抛光造成起的缺陷会随刻蚀时间延长、刻蚀强度增大而消失。经过氢氧等离子体预处理外延生长的单晶中非金刚石相杂质含量较少,结晶性高。     

纳米粉预处理的CVD金刚石薄膜成核与生长研究

研究了纳米金刚石粉预处理的光滑硅衬底上CVD金刚石薄膜的成核与生长．通过与研磨处理样品相比较,纳米金刚石的预处理极大地提高了成核密度（可达10⁹／cm²）、成核速度与成膜质量,并能方便地进行成核密度的控制,是一种经济实用、简单有效的预处理方法．     

石英玻璃上生长表面光滑高光透射率的金刚石膜

石英玻璃衬底在金刚石粉和丙酮形成的悬浮液中超声波预处理,有效提高了金刚石成核密度.在最佳预处理和热丝化学气相沉积条件下,成核密度高达1010 cm-2以上.采用HFCVD中四步法生长工艺,制备出了表面粗糙度小于10 nm、膜厚300 nm、晶粒直径100 nm～150 nm、致密、均匀、高质量和高光透射率的金刚石膜,其1 μm～5 μm波段的光透射率达74%～85%.金刚石膜与石英玻璃衬底结合牢固,膜中无裂纹.     

金刚石纳米粉促进的CVD金刚石薄膜的生长行为研究

采用由普通炸药爆轰制备的金刚石纳米粉对光滑硅衬底进行了涂覆预处理,研究了金刚石薄膜经徐覆和研磨预处理的两种衬底上的生长行为及其演化过程．结果表明,纳米粉处理能在显著提高成核密度的同时,大大缩短长成连续膜所用的时间;薄膜的生长由前后相继的两个阶段所构成,即确定晶面形成前球状颗粒的成长与融合和晶面的逐渐显露与晶粒长大过程．经足够长的生长时间后,所得薄膜具有结构致密、晶面清晰、晶形完整和表面平整度高的特征,特别适合于高致密性自支持薄膜的生长．而研磨处理衬底上生长的薄膜一旦成核,便有确定晶面的显露,但却出现明显的二次成核和孪晶,所得薄膜的致密性与表面平整度均不及徐覆处理的好．文中还对结果进行了简要讨论．     

Mo2C过渡层对金刚石-碳膜场发射均匀性的影响

在经过不同特殊预处理的金属钼衬底上沉积了金刚石 -碳膜 ,分别用X射线衍射谱 (XRD)、拉曼光谱 (Raman)和扫描电子显微镜 (SEM)对样品进行了分析和测试 ,并研究了样品器件的场发射特性。结果发现在金属钼衬底和金刚石 -碳膜之间形成的Mo2 C过渡层与金刚石 -碳膜场发射均匀性有着密切的联系     

采用MPCVD法在硅衬底上选择性生长金刚石膜

采用微波等离子体化学气相沉积（MPCVD）法在附有SiO2掩摸的硅衬底上选择性沉积出了金刚石膜。采用扫描电子显微镜（SEM）和Raman光谱仪对金刚石膜的表面形貌和结构进行了表征。并讨论了衬底温度对金刚石薄膜选择性沉积的影响。得出了较佳的沉积条件。     

Chemical vapour deposition of oriented diamond nanocrystallites by a bias-enhanced nucleation method

A microwave plasma chemical vapour deposition (MPCVD) system has been used to deposit nanometre-sized single-crystalline diamonds on 1 × 1?cm(2) Si(100) substrates. The distribution of deposited diamonds has good uniformity over the whole Si substrate surface by using a dome-shaped Mo anode which allows the application of bias-enhanced nucleation. The morphology and crystallinity of the deposits on Si were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with electron diffraction and lattice images. SEM and TEM observations show that oriented diamond nuclei as single crystals with facets can form on self-formed Si cones through epitaxial SiC within a short bias period. After a longer bias time, it has been observed that polycrystalline diamonds formed as a result of secondary nucleation.     

无支撑、光学级MPCVD金刚石膜的研制

利用引进的6 kW微波等离子体化学气相沉积设备,进行了无支撑金刚石膜工艺的初步研究。在800~1050℃的基片温度范围内,金刚石膜都呈(111)择优取向;基片相对位置对沉积较大面积、光学级金刚石膜至关重要。制出0.25 mm厚Φ50 mm的无支撑金刚石膜。拉曼光谱和X射线衍射分析表明,合成的金刚石膜晶体结构完整,sp2含量极低;透过率测试结果说明了优良的光学性能:截止波长225 nm,光学透过率(λ≥2.5μm)≥70%。     

MPCVD法在氧化铝陶瓷上的金刚石膜沉积及其成核分析

用微波等离子体化学气相沉积（ＭＰＣＶＤ）法在氧化铝陶瓷基片上沉积了金刚石薄膜。实验表明，对基片进行适当的预处理，包括用金刚石研磨膏仔细研磨和沉积前原位沉积一层无定形碳层，可显著提高成核密度；对硅衬底和氧化铝基片上金刚石膜的成核过程进行了对比分析，并提出了提高氧化铝基片上沉积金刚石的成核的措施。     

Si(001)衬底上方形3 C-SiC岛的LPCVD生长

Si衬底上SiC的异质外延生长深受关注,为了了解Si衬底上的成核及长大过程,采用PLCVD方法在Si(001)衬底上生长出了方形3C-SiC岛,利用Nomarski光学显微镜和扫描电子显微镜（SEM）观察了SiC岛的形状,尺寸,密度和界面形貌,结果表明,3C－SiC岛生长所需的Si原子来自反应气源,衬底上的Si原子不发生迁移或外扩散,气相中C原子浓度决定了SiC岛的生长过程。     

MPCVD制备金刚石膜的形核与生长过程

简要介绍了金刚石膜的物理化学特性及应用领域。对比分析了主要化学气相沉积方法的优缺点,并指出MPCVD所面临的技术瓶颈。总结了反应腔体内压强、基片温度、基体材料及增强形核技术对金刚石膜形核过程的影响。较低腔体内压力、基片温度,高碳源浓度及等离子体预处理能有效提高形核密度。阐述了各过程参数对金刚石膜生长的影响和微米、纳米、超纳米金刚石膜的技术特点及应用。指出各类金刚石膜制备所面临的技术难题,并综述了解决该技术瓶颈的最新研究工作。     

CATALYST EFFECT FOR DIAMOND NUCLEATION IN THE LOW PRESSURE PROCESS

The fundamental study of diamond nucleation on several kinds of substrates using the hot-filament CVD method, was carried out. To investigate the diamond nucleation density, the substrate which coated with the catalytic materials by the vacuum deposition was utilized. Diamond particles scarcely grew on a normal Si wafer, but a catalytic material promoted the growth of diamond on the Si substrate. The catalytic material increases the diamond nucleation density as compared with any other substrates with a surface treatment. The particles grown on the substrates have been examined by means of x-ray diffraction and scanning electron microscopy, and identified as diamond.     

Investigation of the nucleation mechanism in bias-enhanced diamond deposition on silicon and molybdenum

Polycrystalline diamond films were deposited on Si and Mo substrates in a microwave plasma-enhanced chemical vapour deposition reactor employing bias-enhanced nucleation. The deposition process was subdivided into two consecutive steps: the pretreatment (bias-enhanced nucleation) and the diamond growth step. To investigate the nucleation process we kept the deposition parameters during the diamond growth step constant and only changed the parameters during the pretreatment. The methods employed to analyze the deposited films after the pretreatment step were electron energy loss spectroscopy (EELS), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy.

The nucleation density (N_D) on Si following the complete deposition cycle (pretreatment and diamond growth step) increases considerably from 5 × 10⁸ cm⁻² to 5 × 10¹⁰ cm⁻² with an increase in the substrate temperature during the pretreatment (T_p) in the temperature range from 680 to 750 °C. For T_p ≥ 770 °C continuous films are formed. The structure of the pretreatment deposit undergoes likewise considerable changes: if T_p exceeds 770 °C the appearance of an intense diamond plasmon at 34 eV is observed, indicative of an increase in the concentration of diamond crystallites embedded in an otherwise amorphous carbon matrix. Our experiments suggest that diamond crystallites formed during the pretreatment serve as nucleation centres for the subsequent diamond growth.

The same deposition parameters which result in the formation of a continuous diamond film on Si, yield only low nucleation densities on Mo. An increase in N_D from 6 × 10⁶ cm⁻² to 2 × 10⁸ cm⁻² can be achieved by raising the methane concentration [CH₄] in the gas phase during the pretreatment from 5 to 50% (T_p = 820 °C). The carbon concentration at the surface for the pretreatment deposit, determined by XPS analysis, increases likewise with [CH₄]. According to the EELS analysis the structure of the pretreatment deposit is comparable with disordered graphite or a-C and no diamond plasmon is observed. The high [CH₄] is required to form the Mo-carbide interface and balance the diffusion of carbon into the metal before the a-C layer can be formed.

The formation of nucleation centres during the bias-enhanced nucleation seems under these deposition conditions to proceed via different pathways on Si and Mo. While the nucleation on Si appears to be linked to the formation of diamond nanocrystals during the pretreatment, this is not the case for Mo.     

Fluidized bed micro-machining and HFCVD of diamond films onto Co-cemented tungsten carbide (WC-Co) hardmetal slabs

The effect of fluidized bed (FB) treatment upon hot filament chemical vapor deposition (HFCVD) of polycrystalline diamond films onto WC-Co hardmetal substrates was investigated. Several scenarios to make the substrates ready for HFCVD were, comparatively, evaluated and the resulting diamond films were examined in terms of their morphology and adhesion. The diamond grain density was measured by scanning electron microscopy. The adhesion of continuous diamond film to substrate was evaluated by the reciprocal of the slope of crack radius-indentation load functions. Surface binder dissolution followed by FB treatment (PF pretreatment) allowed very high diamond nucleation density and smaller grain size. The adhesion of films grown on PF pretreated substrates was found to be very close to that of films deposited on hardmetal slabs pretreated by Murakami's reagent followed by Co etching with Caro's acid and seeded with diamond suspension in an ultrasonic vessel (MPS pretreatment). However, diamond coatings on MPS pretreated samples exhibited a rougher surface morphology as a result of both lower diamond nucleation density and larger substrate surface roughening by Murakami's etching. Based upon experimental findings, our newly developed PF pretreatment was found to be a very promising technique in substrates conditioning as well as in promoting adherent, uniform and smooth diamond coatings onto hardmetal tools and wear parts.