聚醯亞胺-二氧化矽複合材料的合成與耦合劑之研究

Preparation of Polyimide-silica Composites and Study on Coupling Agent

陳威廷(Wei-Ting Chen)

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(2006年)

摘要

本研究以含sulfone基團的二胺單體 (4,4-Diaminodiphenyl sulfone)與二酸酐單體 (3,3’-4,4’-Biphenyltetracarboxylic dianhydride)合成聚醯亞胺，在本研究中將二氧化矽加入聚醯亞胺中目的是為了提升聚醯亞胺的熱性及及機械性質，並添加不同種耦合劑(APrTEOS)與(GOTMS)以改善有機聚醯亞胺與無機二氧化矽之間鍵結，加入二氧化矽以三種方式加入，第一種方式為、藉由溶膠-凝膠法配製四乙基矽烷氧(TEOS)、溶劑(NMP)、水及鹽酸的水解液直接加入聚醯胺酸中；第二種方式以耦合劑3-aminopropyltriethoxysilane (APrTEOS) 加入聚醯胺酸中，再將水解液混合入預先反應形成耦合的聚醯亞胺前驅物；第三種方式將耦合劑γ-glycidyloxypropyltrirn trimethoxysilanes (GOTMS) 與水解液，利用不同方式加入聚醯胺酸中反應形成耦合的聚醯亞胺前驅物。再利用旋轉塗佈法與階段性熱熟化步驟進而得到聚醯亞胺-二氧化矽複合材料。本實驗製備之聚醯亞胺-二氧化矽複合材料採用傅立葉轉換紅外光譜儀(FTIR)、固態矽譜(29Si-solid NMR) 做結構鑑定，化學分析電子儀(ESCA)分析其表面元素組成，SEM觀察其剖面型態，AFM觀察其表面型態，熱機械分析儀TMA、熱重分析儀TGA觀察其熱性質及機械性質。

關鍵字

聚醯亞胺 ； 二氧化矽 ； 溶膠-凝膠法 ； 旋轉塗佈法

並列摘要

In this study, polyimide was prepared by dianhydride 3,3’-4,4’- Biphenyl- tetracarboxylic dianhydride (BPDA) and diamine 4,4-diaminodiphenyl sulfone (DDS) with sulfone group. The silica was added to polyimide in order to enhance the thermal and mechanical property of polyimide. The coupling agent of 3-aminopropyltriethoxysilane (APrTEOS) and 3-glyidyloxyproply trimethoxysilane (GOTMS) were chosen to enhance the bonding between organic polyimide and inorganic silica. The silica was added by three approaches. First, hydrolyzed solution of Tetraethoxysilane (TEOS), 1-Meyhyl-2-pyrrolidine(NMP), DI water and hydrochloric acid for sol-gel reaction was mixed and directly added to poly(amic acid). Second, coupling agent of APrTEOS was added to poly(amic acid), and then mixed with the hydrolyzed solution to form polyimide precursor. Third, GOTMS and hydrolyzed solution was added to the poly(amic acid) to form the polyimide precursor by various ways. Polyimide/silica composites was obtained by spin-coating and multy-step thermal curing process. The structure and surface composite of polyimide-silica composites were characterized by Fourier transform infrared spectrometry (FTIR), 29Si-solid NMR and Electron spectroscopy for chemical analysis (ESCA). The morphology was observed by scanning electron microscopy(SEM) and Atomic Force Microscope (AFM). The thermal and mechanical property was observed by Thermalgravimetric analysis (TGA) and Thermal mechanical analysis (TMA).

並列關鍵字

Polyimide ； Silica ； Sol-gel ； Spin coating

參考文獻

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