预处理工艺对硬质合金与金刚石膜间粘结力的影响

在两种经不同预处理的硬质合金YG8基底上，采用微波等离子体化学气相沉积法，在微波功率2kW，压强4.0kPa和6.5kPa，CH4和H2流量分别为1.6cm/s和100.0cm/s的条件下生长金刚石薄膜。利用X射线衍射检测了金刚石薄膜是否存在，用拉曼光谱分析了薄膜的质量，用金相显微镜观察了薄膜的洛氏硬度压痕，标定并比较了不同预处理工艺膜与基底的结合力。实验结果表明，不同的预处理方法对于粘结力的影响不大，最主要的因素是钴含量的多少。     

Effects of buffer layer materials and process conditions on growth mechanisms of forming networks of SWNTs by microwave plasma chemical vapor deposition

This study investigates the growth mechanism of IC compatible processes and to the feasibility of synthesizing networks of single-walled carbon nanotubes (SWNTs) at lower temperatures (610 °C) on Si wafer using microwave plasma chemical vapor deposition (MPCVD) with CH₄ and H₂ as source gases. The effects of the buffer layer materials (ZnS–SiO₂, Al₂O₃, AlON, and AlN ) and process conditions on growth of carbon nanostructures with Co as catalyst were also examined, where the buffer layers and Co catalyst were deposited in sequence by physical vapor deposition (PVD), followed by H-plasma pretreatment before deposition of carbon nanostructures. Additionally, the morphologies and bonding structures of carbon nanostructures were characterized by field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), and Raman Spectroscopy. Analytical results demonstrate that networks of SWNTs are more favorable to be synthesized by selecting proper buffer layer material (e.g., AlON), and under higher temperatures, thinner catalyst thickness (e.g., 5 nm) and lower CH₄ / H₂ ratio (e.g., 5 / 100 sccm/sccm). The networks of SWNTs can be fabricated at temperatures as low as 610 °C by manipulating these parameters. In conclusion, the growth mechanism determines the conditions for the formation of nano-sized extrusions on catalyst particles surface.     

Effects of Substrate Bias on the Diamond Nanostructure by Reactive Ion Etching

Abstract

Dense and uniform diamond nanocone arrays on titanium substrate were constructed by using bias-assisted reactive ion etching (RIE) of diamond films in a microwave plasma chemical vapor deposition (MPCVD) system. A hydrogen/argon mixture was employed as work gas with ratio of 3/1. The formation of nanocone structure was generated the lengthways physical bombardment/sputtering by argon ions, and selective chemical reaction of graphite and disordered carbons by hydrogen atoms and ions. The structure, size, and density depended on the substrate bias. The surface morphology of diamond film and nanostructures were characterized by field emission scanning electron microscope (FESME), and the composition of diamond film and nanostructures were characterized by Raman spectra. The Stopping and Range of Trons in Matter (SRIM) software was used to simulate the bombardment effect of the diamond film on different Ar⁺ ion incident angles during the etching process. The experimental results showed substrate bias at ?180?V and ?210?V was beneficial to the formation of high density, small size and sharp nanocones, meanwhile larger bias contributed to the formation of large size nanocones. Besides, as-prepared nanocones still maintained significant diamond phase.     

氢气流量对大面积金刚石膜沉积的影响

为了实现大面积金刚石膜的高速均匀沉积,在新型多模微波等离子体装置中,利用微波等离子体(Microwave plasma chemical vapor deposition,MPCVD)技术,对大面积金刚石膜沉积过程中气体流场、电子密度和温度、基团分布及金刚石膜质量进行研究。流场模拟结果表明,多模MPCVD装置在高气体流量下依旧保持良好的流场稳定性。等离子体光谱结果表明,随着氢气流量的上升活性基团的强度上升。氢气流量在400 cm~3/min以内时,活性基团可在基底表面对称均匀分布。电子密度和电子温度随着氢气流量的上升先上升后下降,在500 cm3/min达到最大,分别为2.3×1019/m~3和1.65 eV。在氢气流量为300 cm~3/min时可在直径为100 mm的钼基底上实现大面积金刚石膜的均匀沉积,金刚石膜中心和边缘处拉曼光谱FWHM值为4.39 cm~(-1)和4.51 cm~(-1),生长速率为5.8μm/h。     

MPCVD类金刚石膜抗氧化和摩擦性能的研究

目的研究MPCVD法制备的DLC膜的抗氧化和摩擦性能。方法使用石英钟罩式MPCVD装置,在CH4-H2体系中,通过不同微波功率和沉积气压的正交实验,在载玻片上沉积DLC膜。通过X射线光电子能谱和拉曼光谱对DLC膜表面的化学组成进行测试分析,采用场发射扫描电镜对DLC膜的表面形貌进行观察分析,采用摩擦磨损仪对DLC膜的摩擦性能进行测试研究。结果同一沉积气压下,IO1s/IC1s和sp2/sp3的比值随着微波功率的上升而下降;同一微波功率下,IO1s/IC1s和sp2/sp3的比值随着沉积气压的上升而上升。DLC膜的抗氧化性能随着sp2/sp3比值的下降而上升。场发射扫描电镜结果表明,微波功率由500 W上升至700 W时,DLC膜表面的团聚现象明显受到抑制,摩擦系数下降。当微波功率上升至900 W时,DLC膜表面出现明显裂痕,摩擦系数上升。微波功率为700 W、沉积气压为8.0 k Pa时,可得到氧化性能较好、摩擦系数最低为0.14的DLC膜。结论 MPCVD法制备的DLC膜的抗氧化性能受sp2/sp3比值的影响,比值越低,抗氧化性能越好。摩擦性能同时受sp2/sp3比值和其表面粗糙度的影响,比值越小,表面越平整,摩擦系数越小。     

MPCVD合成P型金刚石薄膜的电导——温度机理

研究了温度对Ｐ型金 石薄膜电导性能的影响，采用微波等离子体化学气相沉积（ＭＰＣＶＤ）的方法在Ｓｉ３Ｎ４基片上制作了掺硼金刚石薄膜，测量了不同掺硼浓度的电导温度特性关系，提出了一种简化的能带模型，解释了电导机理，基于能带模型计算出的电导－－温度关系结果与试验结果相符合。     

MPCVD法在镍基底上低温沉积石墨烯的研究

石墨烯是具有优异性能的二维碳材料。采用微波等离子体化学气相沉积法（MPCVD）,以甲烷和氢气为气源,在镍基底上生长石墨烯薄膜,沉积温度在650℃附近。对制备石墨烯薄膜用金相显微镜、原子力显微镜观察其覆盖率和表面形貌,用拉曼光谱仪对沉积薄膜的层数、质量和非晶碳含量进行表征。研究结果表明氢等离子体对表面碳键有明显刻蚀,产生空隙和晶界缺陷;甲烷含量的升高提高了膜层的覆盖率,也促进非晶碳的生成;气压较低时膜层覆盖率较低,较高时膜层厚度明显增加。     

One-step growth process of carbon nanofiber bundle-ended nanocone structure by microwave plasma chemical vapor deposition

In this work, we report a simple one-step growth process to synthesize a novel and distinct carbon nanostructure, called a carbon nanofiber bundle-ended nanocone (CNFNC) structure, by using microwave plasma chemical vapor deposition (MPCVD) method with CH₄ and H₂ as source gases and Fe catalyst. The nanostructures and their properties after each processing step were characterized by FESEM, HRTEM, ED, AES, and Raman spectroscopy. The preliminary results have demonstrated that the CNFNC structures exhibit excellent field emission properties. The results also show that the favored conditions to form the CNFNC structures include a combination of lower CH₄/H₂ flow ratio, higher substrate negative bias, and proper working pressure and deposition time. The possible growth mechanism of the CNFNC structures is proposed.     

金刚石高成核选择比图形化技术

报道了一种新的金刚石薄膜选择生长图形化技术。首先用直流偏压增强的微波等离子体化学气相沉积（ＭＰＣＶＤ）对图形区域（Ｓｉ）高密度金刚石成核，接着对掩模区域（ＳｉＯ２）进行一次化学浅腐蚀，然后正常生长金刚石薄膜，得到表面光滑、侧壁陡直的金刚石精细图形。用该技术制作了金刚石微马达结构，其厚度为２μｍ，转子直径１５０μｍ。图形间隙可控制至１－２μｍ。     

金刚石聚晶碳膜场发射的场增强特征研究

利用微波等离子体化学气相沉积法(MPCVD),在镀金属钛的纯平陶瓷衬底上制备出一层微米量级的类球状金刚石聚晶颗粒碳膜。通过拉曼光谱仪、X射线衍射仪分析了碳膜的成分,通过扫描电子显微镜观察了碳膜的外部形貌。最后利用场发射的二级结构装置测试了碳膜的场发射性能。讨论了金刚石聚晶碳膜的场发射机理,得出碳膜场发射性能优异的原因是金刚石聚晶碳膜表面存在强大的场增强现象。