新型MPCVD装置的设计及金刚石膜的制备与介电性能研究
发布时间：2018-11-11 20:10
【摘要】：高品质金刚石膜材料在现代技术的各个领域中都有着重要的应用前景。而作为高品质金刚石膜首选的制备方法,微波等离子体化学气相沉积(MPCVD)技术近年来已逐渐走向成熟。但是,相比于美、欧、日等国,我国在高品质金刚石膜的MPCVD制备装备、制备技术方面一直处于落后状态,严重制约了高品质金刚石膜在我国众多高技术领域中的应用。为推动我国MPCVD金刚石膜沉积技术的发展和高品质金刚石膜在各领域中的应用,本文以高功率MPCVD金刚石膜沉积装置的研制入手,继而开展了高功率下高品质金刚石膜制备工艺以及金刚石膜微波介电性能与其质量相互关系的研究。 通过对MPCVD金刚石膜沉积装置谐振腔内等离子体分布、电磁场分布和气体温度分布的数值模拟,本文提出了一种新型穹顶式MPCVD金刚石膜沉积装置。该装置具有以下的优点：(1)石英微波窗口距离等离子体较远,可避免高功率下被等离子体刻蚀的危险；(2)拥有双调谐机制,可以方便有效地实现等离子体分布状态的调节；(3)拥有极佳的真空性能,静态升压法的测试显示,装置的真空泄漏率仅为3.7×10-6Pa·m3·s-1左右；(4)拥有优异的水冷设计系统。实验表明,综合了以上优异性能的新型穹顶式MPCVD装置适合于高微波输入功率下高品质金刚石膜的制备。 在新型穹顶式MPCVD装置成功建立的基础上,本文开展了高品质金刚石膜最优制备工艺的探索,研究了包括沉积温度、甲烷浓度和气体流量三个重要的工艺参数对金刚石膜表面形貌、沉积速率、品质以及取向变化的影响,并研究了装置的真空泄漏率对于高品质金刚石膜制备的影响。研究结果表明,对于新型穹顶式MPCVD装置而言,当沉积温度处于1030℃附近,甲烷浓度处于3.5%附近,气体流量大于100sccm时,最有利于高品质金刚石膜的制备；装置的真空性能会极大地改变金刚石膜的品质,即良好的真空密封性能是MPCVD装置制备高品质金刚石膜的关键之一。但另一方面,装置真空密封性能的改善却会显著降低金刚石膜的沉积速率。 使用新型穹顶式MPCVD装置,在优化的工艺条件下,实现了9.2kW高功率下高品质金刚石自支撑膜的成功制备。检测结果显示,高品质金刚石膜呈现为无色透明状态,光学吸收边约为223nm,其Raman谱金刚石特征峰的半高宽为2.0cm-1,氮杂质含量不足1ppm,在6.5-251μm的红外波段内光学透过率大于70%。这表明,本文制备的金刚石自支撑膜拥有着极高的品质,同时也充分显示了新型穹顶式MPCVD装置在高功率下长时间运行制备高品质金刚石膜的能力。 最后,本文建立了一种分体圆柱谐振腔式低损耗薄膜介电性能测试装置,并对不同质量、不同方法制备的金刚石膜在Ka波段内进行了微波介电性能测试。研究表明,四个金刚石膜(1#、2#、3#和4#的Raman谱半高宽值依次增大,对应的金刚石膜品质依次恶化。随着四个金刚石膜品质的降低,它们的介电常数值依次增大,但其微波介电损耗角正切值却呈现出2#、3#和4#三个样品依次增大,而使用其他分析手段证明的品质较好的1存样品的介电损耗角正切值略高于2#样品的情况。研究表明,1#样品的微波介电损耗角正切值略高于2#样品的原因可能与1#样品的表面存在孔洞和内部存在黑色组织缺陷有关。上述测试结果一方面证明了MPCVD方法制备的金刚石膜可具有较低的介电损耗,同时也证明了金刚石膜的介电损耗与其微观结构密切相关。在今后的研究中,应该对黑色孔洞型缺陷的形成机理、影响因素以及屋顶型孪晶组织对该类缺陷及金刚石膜介电性能的影响展开进一步的系统研究。
[Abstract]:The high-quality diamond film material has an important application prospect in all fields of modern technology. The microwave plasma chemical vapor deposition (MPCVD) technology has gradually become mature in recent years as the first choice for high quality diamond films. However, compared with America, Europe, Japan and other countries, China has been in a backward state in the preparation of MPCVD of high quality diamond film, and has seriously restricted the application of high-quality diamond film in many high-tech fields in China. In order to promote the development of MPCVD diamond film deposition technology in China and the application of high quality diamond film in all fields, this paper starts with the development of high power MPCVD diamond film deposition device. in turn, that preparation technology of high-quality diamond film at high power and the relationship between the microwave dielectric property and the quality of the diamond film are studied. Based on the numerical simulation of the plasma distribution, the electromagnetic field distribution and the gas temperature distribution in the resonant cavity of the MPCVD diamond film deposition apparatus, a new type of top-top type MPCVD diamond film deposition is proposed in this paper. The device has the following advantages: (1) the quartz microwave window is far from the plasma and can avoid the danger of being etched by the plasma at high power; and (2) the device has a double-tuning mechanism, so that the plasma distribution state can be conveniently and effectively realized. and (3) with excellent vacuum performance, the static step-up method shows that the vacuum leakage rate of the device is only about 3. 7-10-6Pa 路 m3 路 s-1; and (4) it has excellent water-cooling design. The experimental results show that the novel top-top type MPCVD device with the above excellent properties is suitable for high-quality diamond films with high microwave input power On the basis of the successful establishment of the new type top-top MPCVD device, the paper studies the optimum preparation technology of high-quality diamond film, and studies the surface morphology of the diamond film by three important process parameters including the deposition temperature, the methane concentration and the gas flow rate. The influence of the deposition rate, the quality and the orientation change is studied, and the vacuum leakage rate of the device is studied for high quality diamond film The results show that, for a new type of top-top MPCVD device, when the deposition temperature is in the vicinity of 1030 鈩，
本文编号：2326000
[Abstract]:The high-quality diamond film material has an important application prospect in all fields of modern technology. The microwave plasma chemical vapor deposition (MPCVD) technology has gradually become mature in recent years as the first choice for high quality diamond films. However, compared with America, Europe, Japan and other countries, China has been in a backward state in the preparation of MPCVD of high quality diamond film, and has seriously restricted the application of high-quality diamond film in many high-tech fields in China. In order to promote the development of MPCVD diamond film deposition technology in China and the application of high quality diamond film in all fields, this paper starts with the development of high power MPCVD diamond film deposition device. in turn, that preparation technology of high-quality diamond film at high power and the relationship between the microwave dielectric property and the quality of the diamond film are studied. Based on the numerical simulation of the plasma distribution, the electromagnetic field distribution and the gas temperature distribution in the resonant cavity of the MPCVD diamond film deposition apparatus, a new type of top-top type MPCVD diamond film deposition is proposed in this paper. The device has the following advantages: (1) the quartz microwave window is far from the plasma and can avoid the danger of being etched by the plasma at high power; and (2) the device has a double-tuning mechanism, so that the plasma distribution state can be conveniently and effectively realized. and (3) with excellent vacuum performance, the static step-up method shows that the vacuum leakage rate of the device is only about 3. 7-10-6Pa 路 m3 路 s-1; and (4) it has excellent water-cooling design. The experimental results show that the novel top-top type MPCVD device with the above excellent properties is suitable for high-quality diamond films with high microwave input power On the basis of the successful establishment of the new type top-top MPCVD device, the paper studies the optimum preparation technology of high-quality diamond film, and studies the surface morphology of the diamond film by three important process parameters including the deposition temperature, the methane concentration and the gas flow rate. The influence of the deposition rate, the quality and the orientation change is studied, and the vacuum leakage rate of the device is studied for high quality diamond film The results show that, for a new type of top-top MPCVD device, when the deposition temperature is in the vicinity of 1030 鈩，
本文编号：2326000
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