等离子体化学气相沉积法及其最新发展

本文将对等离子体的性质、等离子体对化学气相沉积的作用、ＰＣＶＤ反应器以及 新近发展起来的微波等离子体化学气相沉积法（ＭＰＣＶＤ）的特点和应用作一综述。期 望引起国内同行对这一崭新领域的关注，把我国ＰＣＶＤ特别是ＭＰＣＶＤ的研究工 作推向前进。     

等离子体增强化学气相沉积氮化钛薄膜

等离子增强化学气相沉积法(PCVD)是在物理气相沉积(PVD)和化学气相沉积(CVD)基础上发展起来的一种沉积方法。它兼有 PVD 和 CVD 方法的优点。介绍了 PCVD的原理和所研制的一台 PCVD 设备。分析了用 CVD 法和 PCVD 法制备的硬质膜的性能。所分析的性能有:显微硬度、抗弯强度、粘结牢度、机加工性能。     

等离子体化学气相法沉积金刚石薄膜

本文介绍和评述了化学气相沉积法制备人造金刚石薄膜及其进展，重点评述了反应机理，发展历史，沉积方法，补底材料，检测手段，论述了有利于形成立方晶系金刚石材料的沉积条件。     

永磁电子回旋共振等离子体化学气相沉积系统

研制了一台永磁ECR等离子体化学气相沉积系统.通过同轴开口电介质空腔产生表面波,利用高磁能积Nd-Fe-B磁钢块的合理分布形成高强磁场,通过共振磁场区域内的电子回旋共振效应产生大面积均匀的高密度等离子体.进行了ECR等离子体化学气相沉积氧化硅和氮化硅薄膜工艺的研究.6英寸片内膜厚均匀性优于95%,沉积速率高于100 nm/min,FTIR光谱分析表明薄膜中H含量很低.     

等离子体化学气相法沉积金刚石薄膜

本文介绍和评述了化学气相沉积法制备人造金刚石薄膜及其进展。重点评述了反应机理、发展历史、沉积方法、补底材料、检测手段。论述了有利于形成立方晶系金刚石材料的沉积条件。     

微波等离子体化学气相沉积金刚石簿膜

建立了一台微波等离子体化学气相沉积金刚石薄膜的设备。该实验装置由以下几部分组成：微波源及传输系统、反应室、供气系统、真空系统和检测等五部分组成。沉积室是由长７０ｍｍ直径４６ｍｍ的石英管组成的。分别采用ＣＨ４／Ｈ２和ＣＯ／Ｈ２混合气体进行了沉积试验；研究了沉积参数对沉积金刚石膜的影响。在直径３０ｍｍ的单晶硅片和石英片上沉积出了均匀的金刚石膜。采用ＣＨ４／Ｃ２混合气体时，沉积速率在０．５～１．０μｍ／ｈ之间，这与原有的热灯丝方法相近。采用ＣＯ／Ｈ２混合气体时，沉积速率可达到１．７μｍ／ｈ。     

微波等离子体化学气相沉积装置的工作原理

微波等离子体化学气相沉积（ＭＰＣＶＤ）是制备金刚石膜的一种重要方法。用简单实验方法给出了ＭＰＣＶＤ装置中微波模式转换、微波与等离子体耦合等工作原理。矩形波导中的ＴＥ１０模式经微波模式转换器转变为同轴线中的ＴＥＭ模式，再由ＴＥＭ模式转变为圆波导的ＴＭ０１模式。ＴＭ０１模式激发低压气体形成等离子体，等离子体严重影响微波模式分布。在国内首次成功运行了５ｋＷ天线耦合石英窗式ＭＰＣＶＤ装置。     

新型微波等离子体化学气相沉积金刚石薄膜装置

微波等离子体化学气相沉积（ＭＰＣＶＤ）是制备金刚石薄膜的一种重要方法。为了获得金刚石薄膜的高速率大面积沉积，在国内首次研制成功了５ｋＷ带有石英真空窗的天线耦合水冷却不锈钢反应室式ＭＰＣＶＤ装置。初步用该装置成功在硅基片上沉积得到了金刚石薄膜。     

等离子热丝化学气相沉积金刚石膜工艺参数研究

采用等离子热丝化学气相沉积(PHFCVD)装置进行了金刚石薄膜的制备实验。实验条件为：氢气流量为200sccm,甲烷流量为2～12sccm,基体温度为700～900℃,偏压为0～400V,真空室压力为4kPa。通过实验得出了甲烷含量、基体温度和偏压对沉积金刚石膜的影响,并运用扫描电子显微镜(SEM)、原子力显微镜(AFM)和X射线衍射(XRD)等测试方法对金刚石薄膜进行了观察分析。     

工艺参数对化学气相沉积ZrC涂层形貌和组分的影响

利用ZrCl4-Ar-CH4-H2体系,采用化学气相沉积法(CVD)制备了ZrC涂层。研究了不同基底、沉积温度、先驱体中CH4与ZrCl4浓度比(C/Zr)对涂层形貌、物相和组分的影响规律和作用机制。结果表明,不同基底对该体系沉积的ZrC涂层形貌没有显著影响。沉积温度对ZrC涂层形貌影响较大,当温度从1100℃增加到1350℃时,涂层形貌由片状转变到荔枝状,且涂层中的C含量随温度的升高而增加。先驱体中的C/Zr比对涂层形貌和组分也有重要影响,当C/Zr比从8.5减小到3.5时,涂层由疏松多孔形貌经菜花状向玻璃态形貌演变,且涂层中的C含量随C/Zr比的减小而减少。     

Growth of well-aligned carbon nanotubes by RF-DC plasma chemical vapor deposition

Highly aligned carbon nanotubes (CNTs) were grown under high sheath electric field and gas pressure conditions by the radio frequency (RF) plasma-enhanced direct current (DC) plasma chemical vapor deposition (CVD) method due to a stabilized DC discharge. The uniform growth of highly aligned multi-walled CNTs was achieved over the entire surface area of a 50 × 50 mm² iron foil. The growth of multi-walled CNTs on a 75 × 75 mm² iron foil was also confirmed.     

Deposition and characterization of smooth ultra-nanocrystalline diamond film in CH4/H2/Ar by microwave plasma chemical vapor deposition

The smooth ultra-nanocrystalline diamond (UNCD) films were prepared by microwave plasma chemical vapor deposition (MWCVD) using argon-rich CH₄/H₂/Ar plasmas with varying argon concentration from 96% to 98% and negative bias voltage from 0 to −150 V. The influences of argon concentration and negative bias voltage on the microstructure, morphology and phase composition of the deposited UNCD films are investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD), atom force microscopy (AFM), and visible and UV Raman spectroscopy. It was found that the introduction of argon in the plasma caused the grain size and surface roughness decrease. The RMS surface roughness of 9.6 nm (10 micron square area) and grain size of about 5.7 nm of smooth UNCD films were achieved on Si(100) substrate. Detailed experimental results and mechanisms for UNCD film deposition in argon-based plasma are discussed. The deposited highly smooth UNCD film is also expected to be applicable in medical implants, surface acoustic wave (SAW) devices and micro-electromechanical systems (MEMS).     

基于微波等离子体方法生长的纳米碳对碳纤维/环氧树脂复合材料界面性能的影响

为了提高复合材料的界面性能,采用微波等离子体（MPECVD）方法,通过控制工艺参数,在碳纤维（CF）表面生长结构形貌各异的纳米碳,将其引入CF/环氧树脂（EP）复合材料界面微区。采用FESEM研究了不同MPECVD工艺参数对沉积纳米碳结构形貌的影响,采用单纤维破碎实验研究了纳米碳形貌对CF/EP复合材料的界面性能影响,探讨了纳米碳-CF/EP复合材料界面微观结构与其界面性能之间的关系。结果表明：随着MPECVD沉积功率的变化,沉积的纳米碳结构形貌变化较大。当沉积功率为700 W时,制备得到的多尺度纳米碳-CF/EP复合材料界面性能最高,界面剪切强度（IFSS）达到112.38 MPa,提高了118.85%。     

微波等离子体化学气相沉积法在硅片上同时生长碳化硅和金刚石

研究了衬底温度、核化密度、衬底表而预处理等工艺参数对微波等离子体化学气相沉积法在硅片上同时生长碳化硅和金刚石的影响.采用扫描电镜、X-射线衍射、喇曼光谱和红外光谱对样品进行了表征.结果表明:从高核化密度生长的金刚石膜中探测不到碳化硅;不论对硅衬底进行抛光预处理还是未抛光预处理,从低核化密度牛长的金刚石厚膜中总能探测到碳化硅.碳化硅生长在硅衬底上未被金刚石覆盖的地方,或者是在金刚石晶核之间的空洞处.碳化硅形成和金刚石生长是同时发生的两个竞争过程.此研究结果为制备金刚石和碳化砟复合材料提供了一种新的方法.     

Structure control of carbon nanotubes using radio-frequency plasma enhanced chemical vapor deposition

Carbon nanotube structures such as tube diameter, growth site, and formation density are controlled using radio-frequency (RF, 13.56 MHz) plasma enhanced chemical vapor deposition (RF-PECVD) method. We have produced uniformly well-aligned multi-walled carbon nanotubes (MWNTs) grown over the large scale area and linearly arrayed MWNTs grown in a selected area without any highly-sophisticated patterning process. In our RF-PECVD experiment, furthermore, individually grown single-walled carbon nanotubes (SWNTs) or their thin bundles are synthesized for the first time within the scope of the PECVD methods. These results indicate that PECVD method provides the high potential for the further development of nano-technology.     

化学气相沉积法制备无机分离膜

介绍化学气相沉积（ＣＶＤ）法在无机分离膜备方面的应用，以及近期此研究领域的一些进展。     

Texture control of ZnO films by inductively coupled plasma assisted chemical vapor deposition

ZnO films were grown on Si (100) and quartz substrates by inductively coupled plasma-assisted chemical vapor deposition using diethylzinc, O₂, and Ar. ZnO films with the (002) preferred orientation (PO) were formed at substrate temperatures > 250 °C regardless of any other changes made to process variables, since the (002) plane has the lowest formation energy with the highest number of unsaturated Zn-ZnO or O-ZnO bonds. At temperatures < 250 °C, the a-axis plane PO such as (100), (110), and (101) as well as the c-axis (002) plane PO were able to form by varying the temperature, plasma power, and deposition rate. The a-axis PO was formed when the radio frequency power was high enough to produce a crystalline ZnO film but was insufficient to form a (002) PO. The a-axis PO was also formed at higher deposition rates ≥ 20 nm/min when the radio frequency power was high enough to produce crystalline ZnO film. Since the (002) plane grew slowly, the grain exposing (002) plane was overgrown by the grains of the a-axis plane at higher deposition rates.     

Effect of impinging ion energy on the substrates during deposition of SiOx films by radiofrequency plasma enhanced chemical vapor deposition process

Radiofrequency (13.56 MHz) plasma enhanced chemical vapor deposition process is used for deposition of SiO_x films on bell metal substrates using Ar/hexamethyldisiloxane/O₂ glow discharge. The DC self-bias voltage developed on the substrates is observed to be varied from − 35 V to − 115 V depending on the RF power applied to the plasma. Plasma potential measurements during film deposition process are carried out by self-compensated emissive probe. The deposited films are characterized by Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), nanoindentation, nano-scratch test and thermogravimetric analysis. The characterization results show strong dependency of the SiO_x films properties on the energy of the ions impinging on the substrates during deposition. Analysis of Raman spectra indicates an increase in vitreous silica content and reduction in defective Si-O-Si chemical structure in the deposited SiO_x films with increasing ion energy impinging on the substrates. The increase in inorganic (Si and O) content in the SiO_x films is further confirmed from XPS analysis. The growth of SiO_x films with more inorganic content and defect free chemical structure apparently contribute to the increase in their hardness and scratch resistance behavior. The films show higher thermal stability as the energy of the ions arriving at substrates increases with DC self-bias voltage. The possibility of using SiO_x films for surface protection of bell metal is also explored.