本篇論文是利用溶膠-凝膠法製備奈米複合材料以及光子晶體的研究。 在論文的第二章中，以甲基丙烯酸甲酯與甲基丙烯酸-2-羥基乙酯兩種單體與四乙氧基矽烷同時進行高分子聚合以及溶膠-凝膠反應。反應系統藉由適量的起始劑、乙醇、水以及酸觸媒的添加，可以成功的製備出有機-無機奈米複合材料。同時藉由GPC, ASAP, SEM以及TGA等儀器分析得知PMMA/SiO2與PHEMA/SiO2奈米複合材料的熱性質獲得改善。 在論文的第三章中，利用矽以及鋯的氧化物作為殼物質，於其內包覆有機高分子。從研究結果得知如欲獲得氧化矽或是氧化鋯包覆之材質，反應的進行適合在鹼性環境之下操作；當有機高分子表面包覆無機氧化物時，其粒徑約介於0.2~3微米之間，且包覆材料的熱裂解溫度可大幅提昇100℃左右。 在論文的第四章中藉由氣-液界面成功的製造出三維光子晶體以及轉錄型光子晶體結構，從研究結果得知利用氣-液界面不但可以快速的合成光子晶體結構，且由於其具有特定光能隙帶的性質，因此該製程對於光子晶體在未來可作為白光LED與光催化方面的應用。 This study was written to serve as a novel technique to fabricate nano-composite materials and photonic crystals via sol-gel process. In Chapter 2, the organic-inorganic nano-composite materials have been prepared by using methyl methacrylate (MMA), 2-Hydroxyethyl methacrylate (HEMA) and tetraethoxysilane (TEOS) via the sol-gel process. Under the acid condition, 2,2’-azobisisobutyronnitrile (AIBN) was used as the initiator for the polymerization of MMA and HEMA monomer and various amounts of water was added for synthesizing the SiO2 network. It was found that transparent nano-composite materials could be prepared when acid catalyst and appropriate ethanol added into the reaction system. The products were characterized by GPC, ASAP, SEM and TGA thermograms. The results of TGA analysis show that the thermal properties of the PMMA-SiO2 and PHEMA-SiO2 nano-composite materials are improved. In Chapter 3, the organic materials with SiO2 or ZrO2 highly coating microcapsule were successfully prepared in the alkaline condition. The products were characterized by SEM and TGA and DSC thermograms. The heat resistance of the products was improved more than 50℃,and the scale of the products were between 0.2~3 um. In Chapter 4, I propose a novel technique to fabricate a free-standing three-dimensional photonic crystal by self-assembling the colloidal microspheres with controllable thickness from the air–liquid interface. Highly ordered three-dimensional photonic crystals are formed by polymethylmethacrylate or polystyrene monodisperse microspheres. We also demonstrate the fabrication technique of the free-standing inversed opals by removing the microspheres using calcination. The free-standing photonic crystal structures can be used for nano-photonic circuits, white-light LEDs or as a photocatalyst.