自支撑硼掺杂金刚石膜生长及其硼分布、应力的研究
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摘要
本论文采用电子辅助热灯丝化学气相沉积(EA-HFCVD)制备自支撑硼掺杂金刚石膜,对其制备、性质进行了研究。介绍了硼掺杂金刚石膜的生长特性,包括形貌、取向、生长速率等。通过硼掺杂金刚石膜的Raman光谱分析,研究了金刚石膜中硼掺杂相关的Fano干涉现象及硼在膜中的分布情况,即在同等掺杂水平下,(111)晶面的硼掺杂浓度比(110)晶面的大,中心位置的硼浓度高于边界处,晶界处的含硼量高于晶粒;而对于整个自支撑膜来说,表面的硼浓度是最高的。利用XRD(sin2ψ)方法对硼掺杂金刚石膜的应力进行分析,随着硼流量的增加,薄膜的残余应力为压应力,而微观应力经历了拉应力和压应力转化的过程。残余应力和微观应力的变化是由于硼掺杂导致的晶粒尺寸、孪晶生成及(110)和(111)晶面取向变化共同作用的结果。
Diamond is an important material for many applications due to its unique properties such as high hardness, high thermal conductivity, wide band gap (5.5eV), and so on. Pure diamond is known as an insulator. Generally boron doping can induce an acceptor level (p-type semiconductor). Moreover when the boron doping level increased, the metallic conduction even superconductivity will appear. Recently, heavily B-doped (superconductivity) has been investigated extensively.
Freestanding boron-doped CVD diamond films were synthesized by EA-HFCVD process with different B(OCH3)3 flow rates. The growth behavior with different texture, boron concentration, and residual stress of the as grown films were characterized by SEM, XRD and Raman spectra.
Based on the XRD and SEM results, the variation in morphology, grain size and crystalline texture are dependent on the incorporation of boron. The undoped diamond film mainly consists of (111) facet with average size of ~50μm. When boron source was introduced (2 - 10 sccm), the appearance of (110) facets is enhanced with respect to (111) facets and the average size decreases to around 8μm, and importantly, the large number of twin appear. However, as the B-flow rate increased up to 20 sccm, the grains show dominated morphologies of both (110) and (111) facets and the number of twin decreases.
Fano-type interference can be induced by boron doping and the asymmetry parameter q represents the asymmetric of one-phonon line shape which has been proposed that the smaller the q is, the higher the boron concentration is, so we can obtain the distribution of boron by fitting the Raman spectra. The results show that the values of q for (111) facets, grain boundaries and the center of the whole film are smaller than that for (110) facets, grain surface and the edge of the whole film for all the B-doping levels, respectively. This suggests that, at given boron doping levels, (111) facets take up higher concentrations of boron into the crystal than (110) facets, the boron concentration at grain boundaries is higher than that in grain, the boron concentration is higher at center than that at edge. The q increases from top surface to bottom along the cross section, suggesting that the boron concentration near the surface is higher than that beneath.
Generally, doped boron atoms substitute for the carbon atoms and/or occupy neutrally interstitial positions depending on doping level. In these cases, the boron doping leads to stress and consequently influence the structure and properties of those B-doped films. In this paper, the residual and micro stresses were analyzed by XRD. The results show that the residual stress is compressive. With increasing boron flow rate, the stress is gradually decreased. The micro-stress varies as tensile→compressive→tensile in the films fabricated with increasing boron flow rate in the growth processes. It is demonstrated by XRD and SEM that the variations in residual stress and micro-stress as a function of boron doping level are strongly dependent on grain size, growth orientation, and appearance of twins in the boron-doped diamond films. The results are available for designing the high performance diamond-based optoelectronic devices with controlled stress.
Diamond is an important material for many applications due to its unique properties such as high hardness, high thermal conductivity, wide band gap (5.5eV), and so on. Pure diamond is known as an insulator. Generally boron doping can induce an acceptor level (p-type semiconductor). Moreover when the boron doping level increased, the metallic conduction even superconductivity will appear. Recently, heavily B-doped (superconductivity) has been investigated extensively.
Freestanding boron-doped CVD diamond films were synthesized by EA-HFCVD process with different B(OCH3)3 flow rates. The growth behavior with different texture, boron concentration, and residual stress of the as grown films were characterized by SEM, XRD and Raman spectra.
Based on the XRD and SEM results, the variation in morphology, grain size and crystalline texture are dependent on the incorporation of boron. The undoped diamond film mainly consists of (111) facet with average size of ~50μm. When boron source was introduced (2 - 10 sccm), the appearance of (110) facets is enhanced with respect to (111) facets and the average size decreases to around 8μm, and importantly, the large number of twin appear. However, as the B-flow rate increased up to 20 sccm, the grains show dominated morphologies of both (110) and (111) facets and the number of twin decreases.
Fano-type interference can be induced by boron doping and the asymmetry parameter q represents the asymmetric of one-phonon line shape which has been proposed that the smaller the q is, the higher the boron concentration is, so we can obtain the distribution of boron by fitting the Raman spectra. The results show that the values of q for (111) facets, grain boundaries and the center of the whole film are smaller than that for (110) facets, grain surface and the edge of the whole film for all the B-doping levels, respectively. This suggests that, at given boron doping levels, (111) facets take up higher concentrations of boron into the crystal than (110) facets, the boron concentration at grain boundaries is higher than that in grain, the boron concentration is higher at center than that at edge. The q increases from top surface to bottom along the cross section, suggesting that the boron concentration near the surface is higher than that beneath.
Generally, doped boron atoms substitute for the carbon atoms and/or occupy neutrally interstitial positions depending on doping level. In these cases, the boron doping leads to stress and consequently influence the structure and properties of those B-doped films. In this paper, the residual and micro stresses were analyzed by XRD. The results show that the residual stress is compressive. With increasing boron flow rate, the stress is gradually decreased. The micro-stress varies as tensile→compressive→tensile in the films fabricated with increasing boron flow rate in the growth processes. It is demonstrated by XRD and SEM that the variations in residual stress and micro-stress as a function of boron doping level are strongly dependent on grain size, growth orientation, and appearance of twins in the boron-doped diamond films. The results are available for designing the high performance diamond-based optoelectronic devices with controlled stress.
引文
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[16] J Cifre, J Puigdollers, M C Polo, et al. Trimethylboron doping of CVD diamond thin films [J]. Diamond and Related Materials, 1994, 3: 628-631.
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[19] N. Tujimori, H. Nakahata and T. Imai. Properties of Boron-Doped Epitaxial Diamond Films [J]. Japanese journal of applied physics, 1990, 29: 824-827.
[20] M C Polo et al. Comparative study of trimethylboron doping of hot filament chemically vapour deposited and microwave plasma chemically vapour deposited diamond films [J]. Thin Solid Films, 1994, 253(1-2): 136-140.
[21] A W Phelps and R Koba, Proc. I st. Int. Symp. On Diamond and diamond-like Films, 1989, 89(12): 38.
[22]减建兵,黄浩,赵玉成.含搀杂的金刚石[J].金刚石与磨料磨具工程, 2002, 1(127): 17.
[23] Ekimov E A, Sidorov V A. Superconductivity in diamond [J].Letters to nature, 2004, 428: 542-545.
[24] Yoshihiko Takano, Masanori Nagao, Isao Sakaguchi. Superconductivity in diamond thin films well above liquid helium temperature [J]. Appl. Phys. Lett, 2004, 85 (14): 2851-2853.
[25] Li C Y, Li B, LüX Y, Li M J, Wang Z L, Gu C Z. Superconductivity in heavily boron-doped diamond films prepared by electron assisted chemical vapour deposition method [J]. Chinese Phys Lett 2006, 23: 2856-2863.
[26] Vinokur N, Miller B, Avyigal Y et al. Electrochemical Behavior of Boron-Doped Diamond Electrodes [J]. J. Electrochem. Soc., 1996, 143:L238-L240.
[27] Swain G M. The Susceptibility to Surface Corrosion in Acidic Fluoride Media: A Comparison of Diamond, HOPG, and Glassy Carbon Electrodes [J]. J. Electrochem.Soc.,1994, 141: 3382-3393.
[28] Rao T N, Yagi I, Miwa T, et al .Electrochemical Oxidation of NADH at Highly Boron-Doped Diamond Electrodes [J]. Anal. Chem., 1999, 71(13): 2506.
[29] Xu J, Chen Q, Swain G M. Anthraquinonedisulfonate Electrochemistry: A Comparison of Glassy Carbon, Hydrogenated Glassy Carbon, Highly Oriented Pyrolytic Graphite, and Diamond Electrodes [J]. Anal. Chem.,1998, 70(15): 3146.
[30] Chen Q, Swain G M. Structural Characterization, Electrochemical Reactivity, andResponse Stability of Hydrogenated Glassy Carbon Electrodes [J]. Langmuir, 1998, 14(24):7010.
[31] Xu J, Granger M C, Wang J et al. Eletrochemical Society Proceedings, 1999, 99(32): 403.
[32] Troster I, Fryda M, Herrmann D, et al. Electrochemical advanced oxidation process for water treatment using DiaChem (R) electrodes [J]. Diamond Relat . Mater.,2002, 11(3P6): 640.
[33]胡陈果.高硼掺杂金刚石膜电极的电化学应用研究[J].物理学和高新技术, 2002, 31(2): 93-96.
[34]朱沛林,朱建中,杨申仲等.硼掺杂金刚石膜电极电化学特性的研究[J].功能材料与器件学报, 1996, 2(4): 207-214.
[35] Rao T N, Loo B H, Fujishima A, et al. Electrochemical Detection of Carbonate Pesticides at Conductive Diamond Electrodes [J]. Anal chem., 2002, 74: 1578-1583.
[36] Marken F, Paddon C A, Asgan D. Direct cytochrome electrochemistry at boron-doped diamond electrodes [J]. Electrochemistry Communications, 2002, (4): 62-66.
[37] Rao T N, Fujishima A. Recent adrances in electrochemistry of diamond [J]. Diamond and Related Materials, 2000, (9): 384-389.
[38] Lowery S N, Carey J J, Christ C S, et al. Method of electrolysis employing a doped diamond anode to oxidize. US 5 399, 247, 1995.
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