利用主催化劑p-hydroxyphenylacetic acid及助催化劑triethylamine進行低溫亞醯胺化之研究

Abstract

利用主催化劑p－hydroxyphenylacetic acid及 助催化劑triethylamine進行低溫亞醯胺化之 研究 研究生：王俊傑 指導教授：黃華宗博士 國立交通大學材料科學與工程研究所 中文摘要 本研究試將p－hydroxyphenylacetic acid主催化劑及 triethylamine助催化劑與聚醯胺酸混合後，先利用流 變儀量測黏度的變化：在室溫時，隨著p－HPAA濃 度的增加，聚醯胺酸的黏度亦增加，以TEA為催化 劑時，亦有類似的趨勢，但當TEA濃度超過133.3mole ％時，聚醯胺酸會有較低的黏度；在80℃時，添加 過量p－HPAA或TEA之聚醯胺酸會有較低的黏度。 其次進行FTIR低溫亞醯胺化動力學之研究，得知添 加催化劑之聚醯胺酸具有較低的活化能。 最後將添加催化劑之聚醯胺酸旋轉塗佈於silicon wafer及玻璃基材上，完全亞醯胺化後，進行AFM觀 察及機械性質量測、TGA量測、DMA量測。 原子力顯微鏡的觀察顯示添加催化劑使聚亞醯胺薄 膜表面產生突起，催化劑量多，微觀表面愈不平整。 從機械性質量測中，得知添加定量催化劑的聚亞醯胺 ，其應力－應變曲線無明顯變化；添加過量催化劑的 聚亞醯胺，其機械性質變差。從TGA量測中，得知 添加催化劑的聚亞醯胺，其裂解溫度無任何改變。從 DMA量測中，得知添加催化劑的聚亞醯胺，其Tg點 在低濃度時，無明顯的變化，在高濃度時，則轉移至 較低的溫度。 A study on the low temperature imidization with the catalyst p－hydroxyphenylacetic acid and the cocatalyst triethylamine Student：chun-chieh wang Advisor：Dr. Wha-Tzong Whang Institute of Materials Science and Engineering National Chiao-Tung University Abstract In this thesis,we use p-hydroxyphenylacetic acid as a catalyst and triethylamine as a cocatalyst to imidize pol- yamic acid(PAA) at low temperature.The rheology tests (at 25℃)show the viscosity of the PAA increase with the concentration of p-HPAA,and there is a similar case in TEA. But when the concentration of TEA is over 133.3 mole％，the PAA has the lower viscosity.At 80℃, the viscosity of the PAA decrease as the catalyst is over. The kinetic study with FTIR at the low temperature imi- dization shows：the catalysts lower the activation ener- gy of imidization in PAA. Final the PAA was spin-coated and fully imidize on silicon wafers and glass substrates.AFM、the instron、 the TGA、 the DMA were used to characterize the polyimide. The observation of AFM shows that the catalysts make the surface become rough in nanoscale.The higher the cata- lyst content,the rougher the surface. In the tensile-strain tests,the stress and the strain of the PI films change not significant.But as high catalyst con- tent is used in PI,the mechanical properities become wor- se. The datas of TGA show the same thermal stability in spite of the catalyst content. In the DMA tests,the glass-transition temperature of PI does not significantly change at the low catalyst content ,but the glass-transition temperature shifts to the lower temperature at the high catalyst content.