溶膠-凝膠法製備聚醯亞胺-二氧化矽複材之其特性研究

Study on Polyimide-Silicate Hybrids Prepared by Sol-Gel Process

莊坤璋(Kun-Chang Chuang)

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(2005年)

摘要

本實驗以有機單體(BPDA + p-PDA)先合成聚醯胺酸，藉由溶膠-凝膠法將奈米級的SiO2粒子導入聚醯胺酸中，再配合旋轉塗佈及階段性熱熟化步驟奈米合成複合材料。在此研究中SiO2導入基材的目的為提升基材的熱性質。並於聚醯胺酸(PAA)中添加偶合劑(APrTEOS)，藉以改善polyimide與SiO2鍵結。研究中使用傅立葉轉換紅外光譜儀(FTIR)、化學分析電子儀(ESCA)、固態矽譜(29Si-solid NMR)來鑑定其化學結構，熱重損失分析儀(TGA)測定材料的熱穩定性質，(XRD)用來測定材料的結晶性質，(UV/VIS)用來測定材料的透光性，掃描式電子顯微鏡(SEM)用來觀察材料的表面型態。由TGA熱分析的結果顯示聚醯亞胺的二氧化矽添加含量達20%時，其熱裂解溫度提昇20℃。SEM的觀察的結果得知奈米SiO2粒子的顆粒大小約在40~90nm之間。

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. Though a sol-gel process, The silica nano-particles were induced into the PAA precursor. Nanocomposites were obtained from PAA mixture load with silica particles combined with spin coating and multi-step curing process. In this study, silica particles were induced into the PI matrix to promote its thermal properties. The coupling agent 3-aminopropyl
triethoxysilane (APrTEOS) was chosen to enhance the bonding between polyimide(PI) and silica(SiO2). The prepared PI-silica structure were characterized by Fourier transform infrared (FTIR) spectrometry, Electron Spectroscopy for chemical Analysis (ESCA), 29Si - CP MAS solid NMR spectroscopy. The thermal properties, crystallization behavior, and transparency of PI-silica nanocomposites were analyzed by Thermogravimetric analysis (TGA), X-ray diffraction (XRD), and UV-VIS, respectively. The morphology of PI-silica were observed by scanning electron microscopy (SEM). The TGA results indicate that the thermal stability of the nanocomposite can be enhanced by up to 20℃, as silica content increases to 20%.The SEM images show that silica particles with a diameter in the range from 40 and 90 nm.

並列關鍵字

polyimide ； sol-gel ； nanocomposite

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