本研究以合成可用於製備蛋白石結構光子晶體之二氧化鈦空心球為目標，分別嘗試溶膠-凝膠法、植入法以及介面活性劑輔助化學沈澱法，將二氧化鈦披覆於PMMA模板球表面。實驗結果發現，溶膠-凝膠法與植入法所生成之二氧化鈦空心球均勻性不佳，無法應用於排列蛋白石光子晶體。另一方面，利用界面活性劑gelatin B進行PMMA球表面修飾，輔助化學沈澱法則可成功合成出均勻且穩固之二氧化鈦空心球。本研究深入探討介面活性劑輔助化學沈澱法之製程參數影響，包括四氯化鈦水溶液濃度、氨水濃度、反應溫度等，尋求最佳製成條件，獲得均勻分散、粒徑均一之二氧化鈦空心球，並利用不同gelatin B比例本研究可以合成出殼層厚度分別為33 - 49 nm之二氧化鈦空心球。為改善二氧化鈦空心球之表面粗糙度以降低自組裝過程中之摩擦力，使用二氧化矽再包覆二氧化鈦表面，製成滿足光子晶體粒徑均一條件( [ D80 - D20 ] / D50 < 20% )且殼層厚度分別為46 - 56 nm之二氧化鈦/二氧化矽複層空心球。利用等溫誘導加熱自組裝法可成功將二氧化鈦/二氧化矽複層空心球排列成蛋白石光子晶體，由吸收光譜得知，可成功製備出光子能隙波長1679 – 1903 nm的二氧化鈦/二氧化矽複層空心球蛋白石光子晶體，且所得光子晶體之能隙符合理論值，證實製備之樣品確實具有光子晶體之光學特性。

We reported the hard template method with chemical precipitation assisted by gelatin B as surfactant to synthesize uniform and stable TiO2 hollow spheres and expected they can be used to arrange opal structurated photonic crystal. This study thoroughly explored the influence of the process parameters of the surfactant-assisted chemical precipitation method, including the concentration of TiCl4 aqueous solution, the concentration of ammonia, the reaction temperature, and the ratio of gelatin B, etc., and obtained TiO2 shells of different thicknesses. However, the surface of TiO2 hollow spheres is too rough to self-assemble opal photonic crystal. Therefore, in order to improve the surface roughness and reduce the friction force during the self-assembly process, the surface is coated again with SiO2 to form theTiO2/SiO2 hierarchical hollow spheres. Through using the isothermal heating evaporation-induced self-assembly method (IHEISA), we successfully arranged the TiO2/SiO2 hierarchical hollow spheres into opal photonic crystal. The experimental value of the absorption spectrum accorded with the theoretical photonic band gap, confirming that the prepared sample does have the optical properties of photonic crystal.

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