微波ECR等离子体增强溅射制备类金刚石薄膜及沉积过程的等离子体在线诊断
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摘要
本文利用微波电子回旋共振(MW-ECR)等离子体增强非平衡磁控溅射系统,以碳为靶材,氩气为工作气体,制备了类金刚石薄膜。采用拉曼光谱,膜厚测试仪等表征方法研究了不同沉积参数下制备的薄膜的结构成分以及其厚度的变化。
为了研究等离子体参数对薄膜性能的影响,实验中我们使用自行组建的悬浮谐波探针系统对等离子体进行诊断,这种手段有效地克服了探针因表面受到绝缘物污染而失效的问题。实验中,首先对悬浮谐波探针的工作参数进行了优化,在不同的气压下,研究了测试探针偏置电压幅值对悬浮谐波探针的测量结果的影响。改变探针偏置电压的幅值的确会对测量结果产生影响,但是当幅值在3V之内时,各气压下所测得的数据是比较平稳的,并且与单探针的测量结果相符合。然后,在不同微波功率下,通过与单探针测量结果进行比较,验证了悬浮谐波探针测量结果的准确性,悬浮谐波探针测得的电子温度和等离子体密度与单探针的测量结果偏差分别为4.8%和0.08%。最后,对悬浮谐波探针的实用性进行了研究。在薄膜沉积的过程中,尽管探针表面受到绝缘薄膜的污染,其测量结果仍保持不变。这实现了等离子体的在线监控。
此外,使用悬浮谐波探针对不同气压、不同溅射偏压下等离子体的电子温度和等离子体密度进行了测量,并研究了这些参数对所制备类金刚石薄膜性能的影响。
在不同气压下,使用环形碳靶制备了类金刚石薄膜,在0.5Pa时所制备的薄膜的G峰半峰宽最大,且ID/IG值最小。通过调节碳靶上的负偏压,我们发现当偏压绝对值超过500V时,薄膜生长的速率增加,这是本系统存在电压模式和电流模式这两种放电模式所导致的。在靶上的偏压由-400V增大到-650V的过程中,-600V时所沉积的薄膜具有最大的G峰半峰宽和最小的ID/IG值。
In this thesis work, DLC films was prepared by the microwave electron cyclotron resonance (MW-ECR) plasma enhanced unbalanced magnetron sputtering of carbon targets in Ar circumstances. A profiler was used to measure the film thickness, respectively, and Raman spectroscopy was used to study the structure and composition of the film.
In order to observe the relation between the plasma parameters and the film properties, we used the floating harmonic probe technique to measure plasma parameters. It can solve the problem of rapidly failure of the diagnostic tool, i.e. the Langmuir probes, due to surface insulative coating. First, in order to optimize experiment parameters of the floating harmonic probe, we studied the influence of input voltage on the measurement of floating harmonic probe. The voltage amplitude do have certain influence on the measurement results at different pressures,but the data is stable when the amplitude fluctuation is smaller than3V and the data agrees well with the results of Single Langmuir probe. And then, we pay attention to the verification of the accuracy of floating harmonic probe by comparing its measurement results with those from Single Langmuir probe at different input microwave power, As expected, good agreement were received between the floating harmonic probe and single langmuir probe. The measurement represented an accuracy of4.8%, and0.08%with a SLP respectively. Finally, we verified the practicability of floating harmonic probe in the process of thin film deposition. It worked steadily in real circumstance of DLC film deposited, although the surface of the probe was polluted by the insulated films.Monitoring and controlling the process of DLC film deposition can be achieved.
We also measured electron temperature and ion densities at various pressures and sputter voltage, and investigated the influences of these parameters on the quality of DLC films
DLC films deposition is carried out with the carbon target at0.17Pa,0.5Pa,1.0Pa pressure respectively. The film prepared at0.5Pa has the maximum FWHM and the minimum value of ID/IG.When changing the target bias applied on the carbon target, the higher speed of the film deposition appears at-500V. This is identical with the inherent discharge mode (voltage mode and current mode) of the system. In addition, when increasing the bias at the target bias from-400V to-650V, we found that the film deposited at-600V has the maximum FWHM and the minimum value of ID/IG.
为了研究等离子体参数对薄膜性能的影响,实验中我们使用自行组建的悬浮谐波探针系统对等离子体进行诊断,这种手段有效地克服了探针因表面受到绝缘物污染而失效的问题。实验中,首先对悬浮谐波探针的工作参数进行了优化,在不同的气压下,研究了测试探针偏置电压幅值对悬浮谐波探针的测量结果的影响。改变探针偏置电压的幅值的确会对测量结果产生影响,但是当幅值在3V之内时,各气压下所测得的数据是比较平稳的,并且与单探针的测量结果相符合。然后,在不同微波功率下,通过与单探针测量结果进行比较,验证了悬浮谐波探针测量结果的准确性,悬浮谐波探针测得的电子温度和等离子体密度与单探针的测量结果偏差分别为4.8%和0.08%。最后,对悬浮谐波探针的实用性进行了研究。在薄膜沉积的过程中,尽管探针表面受到绝缘薄膜的污染,其测量结果仍保持不变。这实现了等离子体的在线监控。
此外,使用悬浮谐波探针对不同气压、不同溅射偏压下等离子体的电子温度和等离子体密度进行了测量,并研究了这些参数对所制备类金刚石薄膜性能的影响。
在不同气压下,使用环形碳靶制备了类金刚石薄膜,在0.5Pa时所制备的薄膜的G峰半峰宽最大,且ID/IG值最小。通过调节碳靶上的负偏压,我们发现当偏压绝对值超过500V时,薄膜生长的速率增加,这是本系统存在电压模式和电流模式这两种放电模式所导致的。在靶上的偏压由-400V增大到-650V的过程中,-600V时所沉积的薄膜具有最大的G峰半峰宽和最小的ID/IG值。
In this thesis work, DLC films was prepared by the microwave electron cyclotron resonance (MW-ECR) plasma enhanced unbalanced magnetron sputtering of carbon targets in Ar circumstances. A profiler was used to measure the film thickness, respectively, and Raman spectroscopy was used to study the structure and composition of the film.
In order to observe the relation between the plasma parameters and the film properties, we used the floating harmonic probe technique to measure plasma parameters. It can solve the problem of rapidly failure of the diagnostic tool, i.e. the Langmuir probes, due to surface insulative coating. First, in order to optimize experiment parameters of the floating harmonic probe, we studied the influence of input voltage on the measurement of floating harmonic probe. The voltage amplitude do have certain influence on the measurement results at different pressures,but the data is stable when the amplitude fluctuation is smaller than3V and the data agrees well with the results of Single Langmuir probe. And then, we pay attention to the verification of the accuracy of floating harmonic probe by comparing its measurement results with those from Single Langmuir probe at different input microwave power, As expected, good agreement were received between the floating harmonic probe and single langmuir probe. The measurement represented an accuracy of4.8%, and0.08%with a SLP respectively. Finally, we verified the practicability of floating harmonic probe in the process of thin film deposition. It worked steadily in real circumstance of DLC film deposited, although the surface of the probe was polluted by the insulated films.Monitoring and controlling the process of DLC film deposition can be achieved.
We also measured electron temperature and ion densities at various pressures and sputter voltage, and investigated the influences of these parameters on the quality of DLC films
DLC films deposition is carried out with the carbon target at0.17Pa,0.5Pa,1.0Pa pressure respectively. The film prepared at0.5Pa has the maximum FWHM and the minimum value of ID/IG.When changing the target bias applied on the carbon target, the higher speed of the film deposition appears at-500V. This is identical with the inherent discharge mode (voltage mode and current mode) of the system. In addition, when increasing the bias at the target bias from-400V to-650V, we found that the film deposited at-600V has the maximum FWHM and the minimum value of ID/IG.
引文
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[2]Lee K H, Noh S J, Lee B S, el at. Solid-Vapor Equilibrium Phase Diagram of Hydrogen-Adsorbed Carbon[J]. Langmuir,2000,16:10184
[3]Zajickova L, Veltruska K, Tsud N, et al. XPS and ellipsometric study of DLC/silicon interface[J]. Vacuum,2001,61:269
[4]Markus J, Frank V, Voraberger H S, et al. Direct Analysis of Oxidizing Agents in Aqueous Solution with Attenuated Total Reflectance Mid-Infrared Spectroscopy and Diamond-like Carbon Protected Waveguides[J]. Analytical Chemistry,2004,76:384
[5]Hwang M S, Lee C. Effects of oxygen and nitrogen addition on the optical properties of diamond-like carbon films[J]. Materials Science and Engineering B,2000,75:24
[6]顾长志,金曾孙.金刚石膜的性质、应用及国内外研究现状[J].功能材料,1997,28(3)：232-236.
[7]Aisenberg S, Chabor S. Thin Film of Diamond like Carbon[J]. Applied Physics, 1971,42(7):2953.
[8]戴大煌,周克菘.类金刚石薄膜的沉积工艺与应用[M].北京：冶金工业出版社,2001.
[9]Aisenberg S. The role of ion-assisted deposition in the formation of diamond-like carbon films[J]. J. vac. sci. techol.,1990, A8(3):2150-2155
[10]Robertson J. Amorphous carbon thin films[J]. Material science and engineering,2002, 37:129-281
[11]Robertson J. Amorphous carbon[J]. Adv. Phys.,1986,35(4):317-374
[12]Lee S, Park S J, Oh S G. Optical and mechanical properties of amorphous CNfilms[J].Thin Solid Films,1997, (308-309):135-141.
[13]Islli A, Amadatsu S, Minomo S. Characterization of diamondlike carbon films grown
byuper-wide electron-cyclotron resonance plasma ssistedchemical vapordeposition[J] J. Vac. Sci.Technol.,1994,12(4):1068-1073.
[14]Christophe W, Rene G, Louis L. Properties of amorphous carbon films produce by magnetron sputering[J]. Thin Solid Films,1976,32:11-16.
[15]Weissmamel C.Reactive film preparation[J]. Thin Solid Films,1976,32:11-16.
[16]Schroer A, Ensinger W, French G. The properties of amorphous carbonf ilmsobtained by ion-beam-assisted carbon evaporation[J]. Surf. Coat. Technol.,1991,47:418-424
[17]Karabutova A V, Ralchenkoa V G. Comparision of field electron emission from a-C:H films produced by four diferent deposition techniques. [J]. Diamond and Related Materials,1998,17(6):802-806.
[18]Anders S, Anders A, Brown I. Focused injection of vaeuum arc plasmas into curved magnetic filters[J]. J. Appl. Phys.,1994,75(10):4895-4900.
[19]Scheibe H J, Pompe W. Preparation of multilayered film structures by laser arcs [J].Thin Solid Films,1990,193:788
[20]Deshkpandey C, Bunshah R. Diamond and diamond-like films:Deposition processes and properties[J]. J. Vac. Sci. Technol. A,1989,7(3):2294-2300.
[21]Rother B. Estimations and results of energetic condensation processes in relation to hard carbondeposition[J]. J. Vae. Sci. Technol. A,1994,12 (4):1457-1463.
[22]Holland L, Ojha S M. Growth of carbon films with random atomic structure from Ion impaetdamage in a hydrocarbon plasma[J]. Thin Solid Films,1979,58:107-112.
[23]Serra C, Pascual E, Mass F. Plasma deposition of hydrogenated amorphous carbon (a-C:H) under a wide bias potential range[J]. Surf. Coat. Technol.,1991,47:89-96
[24]Nyaiesh A R, Kirby F F, King S F K. New radio frequency technique for deposition of hardcarbon films[J]. J.Vac,Sci.Technol. A,1985,3:610-615.
[25]郭立军,许念坎,刘正堂.射频直流辉光法制备类金刚石薄膜[J].材料研究学报,1994：2：67-73.
[26]Wang Y Y, Wang H Y, Ma G B. Efects of high-temperature annealing on the structure of reactive sputtering a-SiC:H films[J]. Thin Solid films,1998,335:249-252
[27]Jaeob W, Moeller W.On the structure of thin hydrocarbon films Source[J]. Appl. Plays. let.,1993,63(13):1771-1776.
[28]Yoon S F, Rusli,Ahn J, et al. Deposition of polymeric nitrogenated amorphous carbon films (a-C:H:N)using electron cyclotron resonance CVD[J].Thin Solid Films,1999, 340:62-67
[29]刘成龙,杨大智,彭乔.类金刚石薄膜在模拟体液中的电化学阻抗[J].硅酸盐学报,2005,33(11)：1315
[30]朱纪军,左敦稳,王珉.过滤式阴极电弧沉积类金刚石蒲膜工艺研究[J].超硬材料于工程,1998,02：3.
[31]Lettington A H. Appl icat ions of diamond-like carbon thin films[J]. Carbon,1998, 36,5-6:550-560.
[32]丁万昱,高鹏.类金刚石磁盘保护膜的性能、应用与制备[J].真空科学与技术学报,2005,25(01)：41
[33]徐均琪,杭凌伙,惠迎雪.非平衡磁控溅射类金刚石薄膜的特性[J].真空科学与技术学报,2005,25(02)：134
[34]黄卫东.表面波等离子体源合成类金刚石膜及其机理研究(D).合肥：中国科学技术大学2001
[35]桑红毅,张维佳,王天民.类金刚石膜的光学及场发射性能研究现状[J].材料导报,2002,07：38-40
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