基于PCVD法间歇生长模式下纳米金刚石膜的制备研究
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摘要
围绕纳米金刚石膜生长的二次形核理论,我们提出了人工干预诱导二次形核的技术方案,设计出一种通过调解激励电压来改变等离子体激励状态的间歇生长模式。
本文利用直流热阴极PCVD技术,通过微晶金刚石膜传统的连续生长模式生长实验与间歇生长模式实验的对比,研究了人工干预诱导二次形核的机理;并研究了生长和间歇周期、反应压强、温度、缓冲气体及甲烷浓度等参数在直流热阴极PCVD方法间歇生长模式条件下对制备纳米金刚石膜的影响。
研究工作表明,人工干预二次形核由两种因素共同作用导致。工作气压或生长温度的降低,使等离子体激励能量减弱,导致二次形核基团比例增加,成为人工干预二次形核的内在诱因;激励电压的人工调节,导致等离子体能量状况的改变,有利于二次形核行为的引导,同时也会部分增加二次形核基团,成为人工干预二次形核的外在诱因。人工干预的方法,在微晶金刚石膜连续生长模式常用的一些生长条件下,都可以实现二次形核现象的有效诱导,制备出纳米金刚石膜。
通过对相关生长参数的研究,形成了直流热阴极PCVD方法间歇生长模式制备纳米金刚石膜的工艺条件: CH4:H2=(3-5):200 SCCM温度:650-700℃气压:6 kPa(或10 kPa)辅助气体:Ar=20 SCCM(或N2=0.5 SCCM)沉积周期:20-30 min间歇周期:<10 min
人工干预二次形核的提出和间歇生长模式的实验,探索出了制备纳米金刚石膜的新的工艺方法,拓展了直流热阴极PCVD技术的应用范围。
While we understand some of the essential content of second nucleation, an enlightenment is given, so we think an idea to induce second nucleation action by manual adjust, the brief is that we change the state of plasma by adjusting the operating voltage, we name this method intermission mode.
In this paper, using DC hot cathode glow discharge PCVD method, the continue mode and the intermission mode are contrasted, we research the mechanism of second nucleation by manual adjustment , and we research the effect of growth condition, these parameter include the growth and intermission cycle、pressure、temperature、dilution gas and methane concentration.
The result shows that second nucleation by manual inducement is induced by co-action of two factors. The reduction of working pressure or growth temperature, can weaken the energy of excite plasma, this factor is the intrinsic reason of second nucleation by manual inducement; manual adjust of excite voltage can change the state of plasma, this is benefit for guide of second nucleation action, and can increase second nucleation radical, this factor is the external reason of second nucleation by manual inducement. We can implement valid manual inducement of second nucleation and prepare nanocrystalline diamond films at the condition of tradition microcrystalline diamond film growth by the way of manual inducement.
We analysis the experiment samples and have obtained the technics condition of preparation of nanocrystalline diamond films under the intermission mode of DC hot cathode glow discharge PCVD method: CH4: H2=(3-5): 200 SCCM / temperature: 650-700℃/ pressure: 6 kPa(or 10 kPa)/ dilution gas: Ar=20 SCCM(or N2=0.5 SCCM)/ deposition cycle: 20-30 min / Intermission cycle : <10 min.
Second nucleation by manual inducement and the intermission mode, is a novel technics for preparing nanocrystalline diamond film, furthermore it can expand the application field of DC hot cathode glow discharge PCVD method.
本文利用直流热阴极PCVD技术,通过微晶金刚石膜传统的连续生长模式生长实验与间歇生长模式实验的对比,研究了人工干预诱导二次形核的机理;并研究了生长和间歇周期、反应压强、温度、缓冲气体及甲烷浓度等参数在直流热阴极PCVD方法间歇生长模式条件下对制备纳米金刚石膜的影响。
研究工作表明,人工干预二次形核由两种因素共同作用导致。工作气压或生长温度的降低,使等离子体激励能量减弱,导致二次形核基团比例增加,成为人工干预二次形核的内在诱因;激励电压的人工调节,导致等离子体能量状况的改变,有利于二次形核行为的引导,同时也会部分增加二次形核基团,成为人工干预二次形核的外在诱因。人工干预的方法,在微晶金刚石膜连续生长模式常用的一些生长条件下,都可以实现二次形核现象的有效诱导,制备出纳米金刚石膜。
通过对相关生长参数的研究,形成了直流热阴极PCVD方法间歇生长模式制备纳米金刚石膜的工艺条件: CH4:H2=(3-5):200 SCCM温度:650-700℃气压:6 kPa(或10 kPa)辅助气体:Ar=20 SCCM(或N2=0.5 SCCM)沉积周期:20-30 min间歇周期:<10 min
人工干预二次形核的提出和间歇生长模式的实验,探索出了制备纳米金刚石膜的新的工艺方法,拓展了直流热阴极PCVD技术的应用范围。
While we understand some of the essential content of second nucleation, an enlightenment is given, so we think an idea to induce second nucleation action by manual adjust, the brief is that we change the state of plasma by adjusting the operating voltage, we name this method intermission mode.
In this paper, using DC hot cathode glow discharge PCVD method, the continue mode and the intermission mode are contrasted, we research the mechanism of second nucleation by manual adjustment , and we research the effect of growth condition, these parameter include the growth and intermission cycle、pressure、temperature、dilution gas and methane concentration.
The result shows that second nucleation by manual inducement is induced by co-action of two factors. The reduction of working pressure or growth temperature, can weaken the energy of excite plasma, this factor is the intrinsic reason of second nucleation by manual inducement; manual adjust of excite voltage can change the state of plasma, this is benefit for guide of second nucleation action, and can increase second nucleation radical, this factor is the external reason of second nucleation by manual inducement. We can implement valid manual inducement of second nucleation and prepare nanocrystalline diamond films at the condition of tradition microcrystalline diamond film growth by the way of manual inducement.
We analysis the experiment samples and have obtained the technics condition of preparation of nanocrystalline diamond films under the intermission mode of DC hot cathode glow discharge PCVD method: CH4: H2=(3-5): 200 SCCM / temperature: 650-700℃/ pressure: 6 kPa(or 10 kPa)/ dilution gas: Ar=20 SCCM(or N2=0.5 SCCM)/ deposition cycle: 20-30 min / Intermission cycle : <10 min.
Second nucleation by manual inducement and the intermission mode, is a novel technics for preparing nanocrystalline diamond film, furthermore it can expand the application field of DC hot cathode glow discharge PCVD method.
引文
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[2] P. Hartmann, R. Haubner, B. Luk. Deposition of thick diamond films by plused dc glow discharge CVD[J]. Diamond and Related Materials, 1996, 5:850-856.
[3] Y. J. Baik, J.K. Lee, W.K. Lee, et al. Large area deposition of thick diamond films by direct-current PACVD[J]. Thin Solid Film, 1999, 341:202-206.
[4] Lee Joc-Kap, Eun Kwang-Yong, ChaoHee-Baik, et al. Free-standing diamond wafers deposited by multi-cathode, direct-current, plasma-assisted chemical vapor deposition[J]. Diamond and Related Materials, 2000, 9:364-367.
[5] S.H. Kim, Y.S.Park, I.T.Han, et al. Effect of the cyclic growth/etching time ratio on the {100}-oriented texture growth of a diamond film[J]. Thin Solid Films, 1996, 2: 161-164.
[6] J.W.Lee, S.H.Kim, Y.S.Park and I.T.Han. Cyclic technique for the enhancement of highly oriented diamond film growth[J]. Thin solid films, 1997, 303: 264-268.
[7] Y.Hayashi, Y.Matsushita, T.Soga, M.Umeno, et al. Role of cyclic process in the initial stage of diamond deposition during bias enhanced nucleation[J]. Apply Physics, 2002, 91:9752 -9755.
[8] I.U. Hassan, C.A. Rego, N. Ali, W. Ahmed, I.P. O'Hare. An investigation of the structural properties of diamond films deposited by pulsed bias enhanced hot filament CVD[J]. Thin Solid Films, 1999, (355-356): 134-138.
[9]周灵平,李绍禄.CVD金刚石膜表面晶粒度的研究[J].炭素, 1999, 2:17-19.
[10]马丙现,姚宁,杨仕娥等.氢的强化刻蚀对金刚石薄膜品质的影响与SP2杂化碳原子的存在形态[J].物理学报, 2004, 53:2287-2291.
[11] D.M.Bhusari, J.R.Yang, T.Y.Wang, et al. Novel two stage method for growth of highly transparent nano-crystalline diamond films[J]. Chemical Materials Letter. 1998, 36:279-283.
[12] S.T.Lee, H.Y.Peng, et al. Nucleation site and mechanism leading to epitaxial growth of diamond films[J]. Science, 2000, 287:104-107.
[13] P.Hollman, O.Wanstrand, et al. Friction Properties of smooth nanosrystalline diamond coatings[J].Diamond and Related Materials, 1998, (7):1471-1477.
[14]邵乐喜,谢二庆,等.纳米金刚石颗粒涂层的场电子发射[J].兰州大学学报, 1996, 35(2):160-164.
[15] R.Locher, J. Wagner, F. Fuchs, M. Maier, P. Gonon, P. Koidl. Optical and electrical characterization of boron-doped diamond films[J].Diamond and Related Materials, 1995, 4 (5-6):678-683.
[16] Sumio Lijima, Yumi Aikawa and Kazuhiro Baba. Early formation of chemical vapor deposition diamond films[J]. Apply Physics Letter, 1990, 57:2646-2648.
[17] D.M. Gruen, S. Liu, A.R. Krauss,et al. Buckyball microwave plasmas: Fragmentation and diamond film growth[J]. Apply Physics, 1994, 75:1785-1791.
[18] D.M.Gruen. Nanocrystalline diamond films[J]. Annual. Review Materials Science, 1999, 29: 211-259.
[19] D.M. Gruen, S. Liu, A.R. Krauss, J. Luo, X. Pan. Fullerenes as precurors for diamond film growth without hydrogen or oxygen additions[J]. Apply Physics Letter, 1994, 64:1502-1504.
[20] D.M. Gruen, C.D. Zuiker, A.R.Krauss, et al. Carbon dimmer, C2, as a growth species for diamond films from methane/hydrogen/argon microwave plasma[J]. Vacuum Science Technology, 1995, 13:1628-1632.
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