二氧化硅基光导膜的制备及微细加工
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摘要
本文旨在利用溶胶-凝胶法制备性能良好的SiO_2基光导膜，提高膜厚是本文的重点。首先探讨了在传统溶胶-凝胶法制备SiO_2膜的基础上，添加干燥控制剂DCCA，制得SiO_2光导膜；为进一步提高膜厚，探讨了以有机硅氧烷材料和丁氧醇铝为先驱物，制备有机无机复合SiO_2／Al_2O_3光导膜；另外，还研究了厚膜波导光栅的微细加工和紫外激光干涉法制备高密度光栅的新方法。通过光度计测试了薄膜紫外可见吸收光谱和透过率，分析了凝胶膜的感光性；据光度法，计算出光导膜的折射率，分析了折射率随光照和热处理的变化；利用表面轮廓仪测试不同条件下制备的薄膜的厚度；通过红外分光光度计分析了溶胶及薄膜不同条件下的红外吸收曲线；研究发现：
所研究的二氧六环、甲酰氨、草酸以及二甲基甲酰氨四种干燥控制添加剂对SiO_2薄膜均有增厚作用，其中以二氧六环效果最为明显，一次拉膜经500℃热处理后可得到厚度达1.2μm的SiO_2薄膜；
以有机硅氧烷材料(MAPTMS)和丁氧醇铝为先驱物，BzAcH为化学修饰剂，可制备出膜厚度达4.5μm的SiO_2／Al_2O_3复合薄膜；而且这种凝胶膜在325nm附近有明显的吸收峰；用相应波长的紫外光照射这类凝胶膜，随照射时间增加，325nm的吸收峰降低，同时薄膜在有机溶剂中的溶解性发生改变，使薄膜表现出明显的感光性，利用这种感光性可制备出薄膜的微细图形或波导图形；进一步用两束He-Cd干涉激光照射薄膜可制备出线密度为1000条／mm的高密度光栅。
This paper studied on the preparation of the SiO2-based waveguide films by sol-gel process in order to improve the film thickness. DCCA (drying control chemical additive) was added into sols, the SiO2 waveguide films were prepared; To obtain the thicker films, MAPTMS (methacryloxypropyl trimethoxysilane) and Al(O-sec -Bu)a (Aluminum sec-Butoxide) were used as precursors, chemically modified by BzAcH (l-Phenyll-3 -butanedione), the organic-inorganic composite SiO2/Al2C>3 waveguide films were obtained ; Then the fine-pattern of the thicker film and the grating were fabricated using laser interference or UV-irradiation. The absorbance and transmittance spectras were measured by UV-VIS spectre-photometer, by which the photosensitivity of the gel film was analyzed. The refractive index of films and its change with the UV light irradiation or heat-treatment were analyzed. Finally, the film thickness was measured by surface profiler, the FT-IR spectras of the films and the sols were determined by infrar
ed spectrophotometer. The results show that:
Each kind of DCCA, to have been studied on, can help to increase the film thickness, the effect of (CiHO^ is best, using it as DCCA the thickness of the single-layer SiO2 film is about 1.2 u m after heat-treatment at 500癈.
The thickness of the SiO2/Al2O3 film is up to 4.5 u m after heat-treatment at 200癈. Its gel film has the absorption band at around 325nm. So when the gel film was irradiated by the corresponding UV light, the absorption band at 325nm decreases continuously with increasing irradiation time, at the same time, the solubility of the gel film declines in organic solvent, the film shows the good photosensitivity. Due to the good photosensitivity of the gel film , the fine-pattern and the waveguide were obtained. Then when the gel film was irradiated by bi-beam interference, the grating was prepared with the period of around lum.
所研究的二氧六环、甲酰氨、草酸以及二甲基甲酰氨四种干燥控制添加剂对SiO_2薄膜均有增厚作用，其中以二氧六环效果最为明显，一次拉膜经500℃热处理后可得到厚度达1.2μm的SiO_2薄膜；
以有机硅氧烷材料(MAPTMS)和丁氧醇铝为先驱物，BzAcH为化学修饰剂，可制备出膜厚度达4.5μm的SiO_2／Al_2O_3复合薄膜；而且这种凝胶膜在325nm附近有明显的吸收峰；用相应波长的紫外光照射这类凝胶膜，随照射时间增加，325nm的吸收峰降低，同时薄膜在有机溶剂中的溶解性发生改变，使薄膜表现出明显的感光性，利用这种感光性可制备出薄膜的微细图形或波导图形；进一步用两束He-Cd干涉激光照射薄膜可制备出线密度为1000条／mm的高密度光栅。
This paper studied on the preparation of the SiO2-based waveguide films by sol-gel process in order to improve the film thickness. DCCA (drying control chemical additive) was added into sols, the SiO2 waveguide films were prepared; To obtain the thicker films, MAPTMS (methacryloxypropyl trimethoxysilane) and Al(O-sec -Bu)a (Aluminum sec-Butoxide) were used as precursors, chemically modified by BzAcH (l-Phenyll-3 -butanedione), the organic-inorganic composite SiO2/Al2C>3 waveguide films were obtained ; Then the fine-pattern of the thicker film and the grating were fabricated using laser interference or UV-irradiation. The absorbance and transmittance spectras were measured by UV-VIS spectre-photometer, by which the photosensitivity of the gel film was analyzed. The refractive index of films and its change with the UV light irradiation or heat-treatment were analyzed. Finally, the film thickness was measured by surface profiler, the FT-IR spectras of the films and the sols were determined by infrar
ed spectrophotometer. The results show that:
Each kind of DCCA, to have been studied on, can help to increase the film thickness, the effect of (CiHO^ is best, using it as DCCA the thickness of the single-layer SiO2 film is about 1.2 u m after heat-treatment at 500癈.
The thickness of the SiO2/Al2O3 film is up to 4.5 u m after heat-treatment at 200癈. Its gel film has the absorption band at around 325nm. So when the gel film was irradiated by the corresponding UV light, the absorption band at 325nm decreases continuously with increasing irradiation time, at the same time, the solubility of the gel film declines in organic solvent, the film shows the good photosensitivity. Due to the good photosensitivity of the gel film , the fine-pattern and the waveguide were obtained. Then when the gel film was irradiated by bi-beam interference, the grating was prepared with the period of around lum.
引文
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3．张万春．DWDM光纤传输网络的技术发展趋势．光纤与电缆及其应用技术，(6)，2000：16-21．
4. Okamoto K, Takiguchi K, et al. 16-channal potical add/drop multiplexer using silica-based arrayed-waveguide gratings[J]. Electron letter. 31. 1995:723-724.
5. Dana Cristea, F. Craciunoiu, et al. photonic circuitsintegrated with CMOS compatible photodetectors, optical materials, (17), 2001: 201-205.
6．蔡明峻，蔡定平等．光纤通信系统中DWDM技术的近期发展．光电子技术与信息．14(1)．2001：1-10．
7. D.E.Zelmon, H.E.Jackson, et al. A low scattering graded-index SiO_2 planar optical waveguide thermally grown on silicon. Appl. Phys. Lett. 42. 1983: 565-56.
8. J.T. Boyd, R.W. Wu, et al. Guided wave optical structures utilizing silicon. Opt. Eng. 24. 1985: 230-234.
9. O. Grand, J.P. Jadot, et al. low-loss PECVD silica channel waveguides for optical communications. Electron Letter. 26. 1990:2135-2137.
10. D.E.Bossi, J.M.Hammer, et al. Optical properties of silicon oxynitride dielectric waveguides. Appl.Opt, 26, 1987: 609-611.
11. M.kawachi, M.Yasu, et al. fabrication of SiO_2-TiO_2 glass planar optical waveguides by flame hydrolysis deposition. Electron letter. 19. 1983:583-584.
12. A.S.Holmes, R.R.A.Syms et, Fabrication of buried channel waveguides on silicon substrates using spin-on glass, Applied Opt., 32 (25) 1993: 4916-4921.
13. Helmut Schmidt Herbert Krug et al. Development optical waveguides by sol-gel techniques for laser pattering. SPIE (1590). 1991:36-43.
14. R.Reisfeld. prospects of sol-gel technology towards luminescent material. optical material. (16). 2001:1-7.
15．丁星兆，董远达，溶胶-凝胶薄膜工艺及其应用，材料导报，(3)．1998：32-36．
16. D.R Ulrich. Prospects of Sol-Gel processes. Journal of Non-Crystalline Solids. 100.1988: 174～193.
17. J.Zarzycki, M.Prassas, et al. Synthesis of glasses from gels: the problem of monolithic gels. J.Materials Sci. 17. 1982: 3371-3379.
18．沈为民，陈林森．溶胶-凝胶技术在光学制造中的应用．光学技术．(6)，1998：61-65．
19 X.Orignac, R.M.Almeide. Silica-based sol-gel optical waveguides on silicon, IEE Proc. Optoelectron. 143(5). 1996:287-292.
20. R.R.A.Syms, A.S.Holmes. Reflow and burial of channel waveguides formed in sol-gel glass on si substrates. IEEE photonies tech. Lett. 5(9). 1993:1077-1079.
21. Zhai Jiwei, Yang Tao, et al. The optical waveguiding properties of TiO_2-SiO_2composite films prepared by the sol-gel process. Ceramics International. 25. 1999: 667-670.
22. A.Oarcia-Murillo, C.Le Luyer, et al. Elaboration and characterization of Gd_2O_3 waveguiding thin films prepared by the sol-gel process. Optical materials. 16. 2001:39-46.
23．黄元龙，赵光明．溶剂、催化剂对TiO_2溶胶-凝胶过程的影响．功能材料．28(1)．1997：37-41．
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