聚醯亞胺-二氧化鈦和二氧化矽複合材料之合成與性質研究

Synthesis and Characterization of Polyimide/Titania and Silica Hybrid Compodites

葉俊彥(Chun-Yen Yeh)

指導教授 ： 程耀毅

國立臺北科技大學/工程學院/有機高分子研究所/碩士(2008年)

摘要

本研究主要是利用有機單體BPDA與p-PDA 合成聚醯亞胺前驅物聚醯胺酸（PAA），再經由四丁基氧化鈦（TBT）和矽醇鹽（TEOS）進行溶膠-凝膠（sol-gel）反應將奈米級的TiO2 和SiO2粒子導入聚醯胺酸中以形成複合材料，再配合旋轉塗佈及階段性熱熟化步驟得到聚醯亞胺/二氧化鈦和聚醯亞胺/二氧化鈦-二氧化矽複合材料。在此研究中，第一部份將TiO2導入基材的目的是為了探討TiO2對基材熱性質和機械性質的影響，第二部分中將TiO2和SiO2的導入是研究不同比例的無機物對基材的影響。之後使用傅立葉轉換紅外光譜儀（FTIR）、化學分析電子儀（ESCA）來鑑定其化學結構，熱重損失分析儀（TGA）、動態機械分析儀（DMA）和萬能試驗機測定材料的熱性質和機械性質，（UV-VIS）用來測定材料的透光性，掃描式電子顯微鏡（SEM）和穿透式電子顯微鏡（TEM）用來觀察材料的表面型態與二氧化鈦與二氧化矽和基材之間的分散性。由TGA熱分析的結果顯示隨著二氧化鈦的含量增加，其熱裂解溫度會下降。TEM的觀察結果得知二氧化鈦和二氧化矽的顆粒大小在奈米等級。

關鍵字

聚醯亞胺 ； 溶膠凝膠法 ； 奈米複合材料

並列摘要

In this study, two kinds of monomers, 3,3’,4,4’- Biphenyl tetracarboxylic dianhydride (BPDA) and p-phenylenediamine (p-PDA), were employed to synthesize the poly(amic acide) (PAA) precursor of polyimide. Through a sol-gel process of tetrabutyl titanate (TBT) and tetraethoxysilane（TEOS）, the poly（amic acid）/ TiO2 - SiO2 composites was formed. The PI/ TiO2 -SiO2 composites were obtained by a spin coating and multi-step thermal curing process. This resrarch can be divided into two parts. The first part is to mix titanium particles into the PI matrix to study its thermal and mechanical properties. The second part is to investigate the effect of various composition of inorganic oxide in the PI/ TiO2 -SiO2 composites. The structure of prepared hybrid nanocomposite films was characterized by Fourier transform infrared (FTIR) spectrometry, Electron Spectroscopy for chemical Analysis (ESCA). The thermal properties, mechanical properties, crystallization behavior, and transparency of hybrid nanocomposite films were analyzed by Thermogravimetric analysis (TGA), Dynamic mechanical analysis (DMA),Universal Testing Machine,and UV-VIS, respectively. The morphology of hybrid nanocomposite films was observed by scanning electron microscopy (SEM) and transmission electron microscope(TEM). The TGA results indicate that the thermal decomposition temperature of the nanocomposite decreased slightly with increasing TiO2 content. TEM images show that the size of TiO2 and SiO2 particles are with a diameter in nano-scale.

並列關鍵字

polyimide ； sol-gel process ； nanocomposite

參考文獻

[2] I. K. Spiliopovlos, J. A. Mikroyannidis, Macromolecules, 31,1236(1998)

[5] J.C Jung, S.B. Park, J. Polym. Sci, Part A: Polym Chem., 34,357(1996)

[6] W. Hatke, H.W. Schmitz, W. Heitz, J Polym Sci, Part A:Polym Chem. ,29,1387(1991)

[10] G. Philipp, H. Schmidt, J. Non-Cryst Solids, 63,283(1984)

[14] B.M. Novak, ADvanced Materials, 5(6),629(1993).