用不同溅射方法镀制SiO_2薄膜光学特性的研究
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摘要
二氧化硅(SiO2)薄膜的折射率低、消光系数低、色散小、附着力强、粗糙度小,在可见光和近红外区域均为透明,是一种理想的光学薄膜。另外,SiO2薄膜的硬度大、绝缘性好、耐磨损、抗腐蚀、化学性能稳定,抗激光损伤阈值较高,机械性能优越,已经广泛地应用于光学、机械及微电子等领域。随着近年来大功率激光器的发展,特别是大功率激光器在武器中的应用,人们对SiO2薄膜的抗激光损伤特性表现出了极大的兴趣。
目前制备SiO2薄膜的方法很多,其中反应磁控溅射(RMS)和离子束反应溅射(RIBS)方法是目前国内外高度重视的镀膜方法。本文用这两种方法制备了SiO2薄膜。采用椭偏仪测试并分析了薄膜的光学性能。测试表明：工作气体中O2含量在大于16%时通过RMS法沉积的SiO2薄膜在630nm波长处折射率约为1.46-1.5,消光系数低于10-5。用RIBS沉积SiO2薄膜氧气含量大于80%时,制备的SiO2薄膜在波长为630nm处的折射率在1.45-1.47之间,薄膜在很宽的波长范围内透明,薄膜的消光系数低于10-5。采用X射线光电子能谱(XPS)测试RMS最优条件制备的SiO2薄膜,氧硅比为2.05:1。采用1-on-1方式测试了薄膜对1064nm激光的抗激光损伤阈值,本文中RMS方法制备的SiO2薄膜阂值最高达到8.89J/cm2, RIBS方法沉积SiO2薄膜阈值最高达到25.01J/cm2。
实验表明,磁控溅射方法和离子束溅射法均可以制备出和块体材料相近折射率、低消光系数的SiO2薄膜。采用磁控溅射时最佳工艺参数为：恒流模式IT=0.7A(Pt=0.3kW),氩气流量为65 sccm,氧气流量22sccm。采用离子束溅射时最佳工艺为U=3.7KV,I=120mA,氧气流量20sccm。
Silicon oxide (SiO2) thin film is an ideal optical material for its low refractive index, low extinction coefficient, small dispersion, strong adhesion, small surface roughness and high transmission in visible and near infrared region; meanwhile, the mechanical properties of silicon oxide thin film are also outstanding, such as high hardness, chemical inert, high abrasive corrosion resistance and high laser induced damage threshold. So the SiO2 thin film is widely used in optics, mechanical manufacture and microelectronics. At present, the SiO2 thin film attracts more attention in the development of high power laser and especially in the laser weapon for its high laser induced damage threshold.
There are many methods to deposit SiO2 thin film. The reactive magnetron sputtering (RMS) and reactive ion-beam sputtering (RIBS) deposition are recognized as the main methods for preparing SiO2 thin film. In this paper, SiO2 thin film was deposited on stainless successfully by RMS and RIBS deposition to improve its characteristics.
The optical properties of SiO2 thin film were measured by spectroscopic ellipsometer. The results showed that when the O2 content in working gas mixture more than 16%, the refractive index of SiO2 film deposited by RMS was 1.46～1.5 at 630nm wavelength and the extinction coefficient was less than 10"5. When the O2 content in working gas mixture more than 80%, the refractive index of SiO2 film deposited by RIBS was 1.45-1.47 at 630nm wavelength and the extinction coefficient was less than 10-5. The analysis of the XPS prove that the stoichiometry of silicon oxide was 2.05. By 1 on 1 test method, when the laser wave was 1064nm, the laser induced damage threshold of the film deposited by RMS was 8.89J/cm2, the laser induced damage threshold of the film deposited with RIBS was 25.01 J/cm2.
The experiments showed that RMS and RIBS deposition could deposit SiO2 thin film with low refractive index and low extinction coefficient. The optimal technological parameters of the RMS were described as follows:the current was 0.7A, the flow rate of Ar was 65sccm, and the flow rate of O2 was 22sccm. The optimal technological parameters of the RIBS were described as follows:the voltage was 3.7KV, the current was 120mA, and the flow rate of O2 was 22sccm.
目前制备SiO2薄膜的方法很多,其中反应磁控溅射(RMS)和离子束反应溅射(RIBS)方法是目前国内外高度重视的镀膜方法。本文用这两种方法制备了SiO2薄膜。采用椭偏仪测试并分析了薄膜的光学性能。测试表明：工作气体中O2含量在大于16%时通过RMS法沉积的SiO2薄膜在630nm波长处折射率约为1.46-1.5,消光系数低于10-5。用RIBS沉积SiO2薄膜氧气含量大于80%时,制备的SiO2薄膜在波长为630nm处的折射率在1.45-1.47之间,薄膜在很宽的波长范围内透明,薄膜的消光系数低于10-5。采用X射线光电子能谱(XPS)测试RMS最优条件制备的SiO2薄膜,氧硅比为2.05:1。采用1-on-1方式测试了薄膜对1064nm激光的抗激光损伤阈值,本文中RMS方法制备的SiO2薄膜阂值最高达到8.89J/cm2, RIBS方法沉积SiO2薄膜阈值最高达到25.01J/cm2。
实验表明,磁控溅射方法和离子束溅射法均可以制备出和块体材料相近折射率、低消光系数的SiO2薄膜。采用磁控溅射时最佳工艺参数为：恒流模式IT=0.7A(Pt=0.3kW),氩气流量为65 sccm,氧气流量22sccm。采用离子束溅射时最佳工艺为U=3.7KV,I=120mA,氧气流量20sccm。
Silicon oxide (SiO2) thin film is an ideal optical material for its low refractive index, low extinction coefficient, small dispersion, strong adhesion, small surface roughness and high transmission in visible and near infrared region; meanwhile, the mechanical properties of silicon oxide thin film are also outstanding, such as high hardness, chemical inert, high abrasive corrosion resistance and high laser induced damage threshold. So the SiO2 thin film is widely used in optics, mechanical manufacture and microelectronics. At present, the SiO2 thin film attracts more attention in the development of high power laser and especially in the laser weapon for its high laser induced damage threshold.
There are many methods to deposit SiO2 thin film. The reactive magnetron sputtering (RMS) and reactive ion-beam sputtering (RIBS) deposition are recognized as the main methods for preparing SiO2 thin film. In this paper, SiO2 thin film was deposited on stainless successfully by RMS and RIBS deposition to improve its characteristics.
The optical properties of SiO2 thin film were measured by spectroscopic ellipsometer. The results showed that when the O2 content in working gas mixture more than 16%, the refractive index of SiO2 film deposited by RMS was 1.46～1.5 at 630nm wavelength and the extinction coefficient was less than 10"5. When the O2 content in working gas mixture more than 80%, the refractive index of SiO2 film deposited by RIBS was 1.45-1.47 at 630nm wavelength and the extinction coefficient was less than 10-5. The analysis of the XPS prove that the stoichiometry of silicon oxide was 2.05. By 1 on 1 test method, when the laser wave was 1064nm, the laser induced damage threshold of the film deposited by RMS was 8.89J/cm2, the laser induced damage threshold of the film deposited with RIBS was 25.01 J/cm2.
The experiments showed that RMS and RIBS deposition could deposit SiO2 thin film with low refractive index and low extinction coefficient. The optimal technological parameters of the RMS were described as follows:the current was 0.7A, the flow rate of Ar was 65sccm, and the flow rate of O2 was 22sccm. The optimal technological parameters of the RIBS were described as follows:the voltage was 3.7KV, the current was 120mA, and the flow rate of O2 was 22sccm.
引文
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[3]邵淑英,范正修,邵建达,等.氧分压对电子束蒸发SiO2薄膜机械性质和光学性质的影响[11].光子学报,2005,34(5)：742-744
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[7]冯涛.光学薄膜离子束辅助蒸发沉积技术新进展[J].今日科苑,2010,25(14)：37-41.
[8]Hubler G.K. Fundamentals of ion-beam-assisted deposition:technique and film properties[J].Mater. Sci. and Engin,1989,A115(1):181-192.
[9]Haruo Takashashi. Temperature Stability of Thin film Narrow band pass Filters Produced by Ion assisted Deposition[J].Applied Optics,1995 (34):667-675.
[10]黄志强,倪宏伟,徐政,等.基片掺杂与热氧化Si02薄膜驻极体的电荷贮存特性[J].功能材料,1999,30(5)：500-502.
[11]Seifarth H, Grotzschel R, Markwitz A,et al. Preparation ofSiO2 with embedded Si manocrystals by reactive R.F. magnetron sputtering [J].Thin Solid Films,1998, 330(1):202-205.
[12]Tomozeiu N., van Hapert J. J., van Faassen E. Structural properties of a-SiOx layers deposited by reactive sputtering technique [J].Optical. and Advanced Mater,2002,4(3):513-521.
[13]Tomozeiu N., SiOx thin films deposited by r.f. magnetron reactive sputtering:structural properties designed by deposition conditions [J].Optoel. and Advanced Mater,2006,8(2):769-775.
[14]茅听辉,陈国平,蔡炳初.反应磁控溅射溅射的进展[J].真空,2001,8(4)：1-2.
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[16]刘玉荣,李观启,黄美浅.用IR及XPS研究Photo-CVDSiO2薄膜特性[J]Journal of South China Universitu of Technology,2003,31(7):61-64.
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