溶胶-凝胶技术制备有机-无机复合平面波导薄膜
文献类型：学位论文
| 作者 | 王宝玲 |
| 学位类别 | 博士 |
| 答辩日期 | 2005 |
| 授予单位 | 中国科学院上海光学精密机械研究所 |
| 导师 | 胡丽丽 |
| 关键词 | 溶胶－凝胶 复合膜 有机改性硅酸盐 平面波导 光学性质 |
| 其他题名 | Hybrid inorganic-organic planar waveguide film prepared by sol-gel method |
| 中文摘要 | 完整的集成光学系统是由多种有源和无源器件构成。平面光波导是制备各种集成光学器件的基础。由于传统的溶胶一凝胶法在制备纯无机物薄膜时具有一些局限性，如单层膜厚较小（几百纳米）、厚膜容易开裂等，而平面光波导一个最基本的要求是膜厚较大（几个微米），这样就使平面光波导薄膜的制备增加了一定的难度。有机一无机复合材料的出现有效解决了这种传统溶胶一凝胶法的弊端。本论文采用溶胶一凝胶法制备了TiO2/ormosil、ZrO2／ormosil和ZnO／ormosil三个系统的有机一无机复合平面波导膜和染料掺杂复合膜，利用红外光谱仪、紫外一可见光谱仪、荧光光谱仪、原子力显微镜、扫描电镜、热分析仪、棱镜耦含法、显微硬度计和粘度计等测试方法研究了制备工艺，包括有机、无机前驱物配比、力日水量、溶剂加入量、溶胶老化时间以及热处理温度等对薄膜结构及光学性质的影响。论文首先选取了丫一缩水甘油醚基丙基三甲氧基硅烷（GLYMO）和三甲氧基硅烷丙基丙烯酸酯（TMSPM）两种典型的有机硅烷作为制备有机一无机复合膜的前驱物，比较了二者在溶胶制备、复合膜结构和性质方面的差别。实验结果表明，在相同制备条件下，选用GLYMO制备的复合膜品质优于TMSPM，从而确定采用GLYMO作为制备复合波导膜的有机前驱物。论文着重研究了Ti02／GLYMO复合膜的制备和性质。实验结果表明，150℃热处州2h即可获得透明、致密且较硬的薄膜。溶胶在不同的一老化时间内。可得锂膜 享0.307-16．11μm，折射率1．53一1．55（632．8nm）的单层膜；在632．8mmI波长下，平面波导损耗小于ldB／cm，实验得出，起始溶胶中前驱物摩尔百分比为GLYMO：Ti（OBu）4：80％：20％，老化3天所制备的复合膜品质最优。低温热处理对TiO2／GLYMO复合膜中染料的光谱性质产生了不同的影响，随着热处理温度升高，RB、R6G、PM567和PM597的荧光光谱强度降低，吸收和荧光峰位不变。但是kitonred的荧光光谱强度明显增加，并且吸收和荧光峰位蓝移。沦文中还对S1O2／TiO2／GLYMO三元复合膜作了研究，结果表明，不同的溶胶加水量使SiO2／TiO2／GLYMO三元复合膜的折射率和厚度不同，并且随着加水量增加，薄膜表面粗糙度增大，损耗变大，而且过量的加水量还会引起复合膜透光率大大下降。论文对ZrO2／GLYMO复合膜作了简单研究。实验结果表明，当溶剂添加量较多时，复合膜折射率和厚度都较小，透光率较高，传输损耗增大。TiO2／GLYMO复合膜与之相比具有较小的传输损耗。rO2／GLYMO复合膜中染半粕勺吸收和荧光性质与TiO2／GLYMO复合膜具有相似的结果：论文最后初步探索了ZnO／GLYMO复合膜的制备工艺。实验结果表明，采用三水合乙酸锌和GLYMO可以制备出无色、透明、丧面光滑上无裂纹的ZnO／GLYMO复合膜。但是复合膜折射率较低，不适合在载波片上形成平面波导。 |
| 英文摘要 | A system of integrated optics consists of many passive and active components. Planar waveguide is one of those components. There are some defects such as smaller thickness of single-layer coating (several hundred nanometer), crack of thicker film in the traditional sol-gel method. But a pre-condition of planar waveguide is its thickness (several micron). Therefore, it is difficult to prepare thicker planar waveguide film by the traditional sol-gel method. The appearance of hybrid inorganic-organic material solves these problems. In this dissertation, hybrid TiCb/ormosil, ZrCb/ormosil, ZnO/ormosil planar waveguide films and dye-doped hybrid films have been prepared by the sol-gel method. The influence of processing parameters including the molar ratios of inorganic and organic precursors, water and solvent content, sol aging time and heat-treatment temperature on the structural and QptlfflSl properties was investigated. The properties of films were measured VrtHS" j^aflning electron microscopy, UV/VIS/NIR spectrophotometer, "WMiMi0MOisteT. FP-6500 spectrofluorometer, atomic force microscopy, thermal analysis instrument, m-line, the scattering-detection method, rotation viscometer and m&rd-hardness meter. The results indicate: under the same condition, the quality of TiCVGLYMO film is better than that of TiCb/TMSPM film. For the TiO2/GLYMO film, transparent, dense and hard film can be obtained after heat-treatment at 150 °C for 2h. The thickness of 0.307-16.11 u m and the refractive index of 1.53-1.55 ( 632.8nm) were obtained in the single-layer film within the different sol aging time. The propagation loss of the planar waveguide films was lower than ldB/cm (632.8nm). In this work, the waveguide films prepared from sol with molar ratio of GLYMO: Ti(OBu)4=80%: 20% and sol aged for 3 days have the best optical qualities. Low heat-treatment temperature has different effect on the spectral properties of dye-doped TiCVGLYMO films. With the increase of temperature, the fluorescence intensity of RB, R6G, PM56 and PM597 decreases, and no peak shift in the absorption and emission spectra. However, the fluorescence intensity of kiton red increased obviously, and blue-shift of peaks was observed. For the SiCVTiCVGLYMO film, with the increasing water content in sol, the surface roughness and propagation loss increase, excess water content causes lower transmittance. For the ZrCh/GLYMO film, smaller thickness and refractive index, higher transmittance and optical loss were found with more solvent content in sol. As compared with TiOi/GLYMO film, the optical loss of ZrOi/GLYMO film is larger. The absorption and emission spectra of dye-doped ZrO2/GLYMO film is the same as the results of dye-doped TiCk'GLYMO film. Colorless, transparent, smooth and crack-free hybrid ZnO/GLYMO film can be prepared by zinc acetate dihydrate and GLYMO, but the refractive index of film is too low to form the planar waveguide on the soda-lime glass substrate. |
| 语种 | 中文 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/15391]  |
| 专题 | 上海光学精密机械研究所_学位论文 |
| 推荐引用方式 GB/T 7714 | 王宝玲. 溶胶-凝胶技术制备有机-无机复合平面波导薄膜[D]. 中国科学院上海光学精密机械研究所. 2005. |
入库方式： OAI收割
来源：上海光学精密机械研究所
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