摘 要 本實驗是藉由溶膠-凝膠(Sol-Gel)法,在高濃度的無機酸(HCl)存在下來溶解易快速沉降的二氧化鈦粉體,以有效取代螯合劑來控制鈦醇鹽類的反應速率, 來製備聚亞醯胺/二氧化鈦有機-無機混成材料。 實驗利用溶膠-凝膠(Sol-Gel)法,將無機氧化物-二氧化鈦(TiO2)的前驅體Ti(OC4H9)4與偶合劑(Coupling Agent)APrTMOS製備成一無機聚合物,再將此無機聚合物導入以4,4-oxydianiline (ODA)和4,4-oxydiphthalic anhydride(OPDA)單體合成的聚亞醯胺酸中,隨後在高溫下進行環化反應合成聚亞醯胺,並同時促進溶膠-凝膠(Sol-Gel)的縮合反應,製備成聚亞醯胺/二氧化鈦有機-無機混成材料。 實驗中針對所製備的混成材料薄膜的結構、表面型態、熱性質分析、光學性質、機械性質、介電等,做了初步的性質測試。以IR做初步的結構比對鑑定,DSC,TGA等探討有機-無機混成薄膜的熱性質,TEM,SEM觀察無機物(TiO2)在聚亞醯胺(Polyimide)基材中的分散性及顆粒粒徑大小,DMA觀察其機械性質,光學性質之UV-Vis分析, 阻氣性質分析(GPA) ,吸水性質。 實驗結果由TEM觀察證實,所製備的聚亞醯胺/二氧化鈦有機-無機混成材料薄膜,其無機物的微粒均勻分佈於聚亞醯胺基材中,平均 粒徑約為50nm(PI-5%)。實驗測得聚亞醯胺熱裂解溫度大約591℃,於添加少量TiO2時,聚亞醯胺混成材料熱裂解溫度在602℃,大約提升10℃~11℃。隨著(TiO2)含量增加,聚亞醯胺熱裂解溫度反而下降到593℃。光學性質亦隨著無機(TiO2)含量的增加而隨之變化。就阻氣、吸水性質方面而言,亦因(TiO2)的增加而些微提升了材料阻氣及降低吸水的效果。介電常數亦隨無機物的加入而下降。
Abstract In this dissertation, a series of polyimide-titania (PI-TiO2) hybrid materials were successfully prepared under the incorporation of high inorganic acid concentration (without chelating agent) through conventional thermal imidization reactions. Typically, 4,4-diaminodiphenyl ether (ODA) and 4,4-Oxydiphthalic anhydride (OPDA) were used as diamine and dianhydride, respectively, to play the role for the organic component. On the other hand, titanium(IV)n-butoxide (TBT) and AprTMOS (3-Aminopropy 1-trimethoxysilane) were used as inorganic sol-gel precursor and coupling agent, individually. The as-prepared hybrid materials were subsequently characterized by Fourier-Transformation infrared (FTIR) spectroscopy, transmission electron microscopy (TEM) and atomic force microscopy (AFM). The experimental results demonstrated the thermal, mechanical, gas barrier properties and optical clarity of hybrid materials were improved relative to pure PI based on the studies of thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), gas permeability analyzer (GPA) and UV-visible transmission spectroscopy.