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研究生: 黃威浤
Huang, Wei-Hung
論文名稱: 對排/同排聚苯乙烯摻合體結晶行為之研究
Crystallization behavior of syndiotactic/isotactic polystyrene blends
指導教授: 王紀
Wang, Chi
學位類別: 碩士
Master
系所名稱: 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年: 2007
畢業學年度: 95
語文別: 中文
論文頁數: 136
中文關鍵詞: 相溶性聚苯乙烯結晶快速傅立葉轉換
外文關鍵詞: crystallization, miscibility, polystyrene, Fast Fourier Transform
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  • 本研究將對排聚苯乙烯(sPS)/同排聚苯乙烯(iPS)混摻於熔融態以phase contrast OM觀察相分離隨時間變化,並將影像經FFT轉換,可計算出domain與domain的間距Λ,且隨時間變化可求得coarsening速率。並利用enthalpy relaxation以及SEM探討相溶性。sPS/iPS=50/50與sPS/iPS=30/70混摻於熔融態等溫不同時間後quench,在sub-Tg回火12小時,由DSC第一次升溫曲線可得一個recovery peak,但在150oC出現多個冷結晶峰,隨著於熔融態等溫時間增加,最後只剩下一個冷結晶峰。而由SEM影像,並沒有發現會相分離成兩層的情況。

    利用SALS與POM量測sPS/iPS混摻冷結晶晶體成長速率,且觀察成長過程,發現於熔融態等溫不同時間後quench,冷結晶時iPS的晶體成長速率並不相同,且不同於sPS/aPS混摻,無法觀察到冷結晶時sPS的晶體成長。

    Syndiotactic polystyrene / isotactic polystyrene blends were examined by phase contrast OM to study the changes of phase separation with time. The OM image, converted by FFT, helped to calculate the distance Λbetween domains and to determine the coarsening rate. Enthalpy relaxation and SEM were also used to explore the blend miscibility. Recovery peaks could be observed form the first DSC heating scan for the sPS/iPS=50/50 and sPS/iPS=30/70 blends, which were held at 300oC for various times, and quenched to room temperature, followed by sub-Tg annealing at 75oC for 12 hours. Multiple cold crystallization peaks appeared for short time residence of 300oC while only one cold crystallization peak was observed with the prolonged holding time at 300oC. Based on the SEM images, it was not found that phase separation was separated into two layers.

    SALS and POM were used to observe the growth process to measure the growth rate of the iPS in the blends during cold crystallization at low temperatures. It was found, after quenching of the melting status (isotherm with different period), that the crystal growth rate of iPS in cold crystallization is different from sPS/aPS blends, and thus it is impossible to observe the crystal growth of sPS in the blend.

    目錄 中文摘要…………………………………………………………………i 英文摘要………………………………………………………………ii 誌謝……………………………………………………………………iii 目錄……………………………………………………………………iv 圖目錄…………………………………………………………………vii 符號…………………………………………………………………viii 一、前言…………………………………………………………………1 二、簡介…………………………………………………………………2 三、文獻回顧……………………………………………………………3 3.1 對排聚苯乙烯…………………………………………………3 3.2 同排聚苯乙烯…………………………………………………6 3.3 聚苯乙烯之摻合體……………………………………………8 3.4 相分離………………………………………………………10 四、理論………………………………………………………………17 4.1 高分子摻合體相溶性………………………………………17 4.1.1 高分子摻合系統熱力學性質…………………………17 4.1.2 兩成分系高分子摻合體相圖…………………………19 4.1.3 Kinetics of phase separation …………………20 4.2 SALS理論……………………………………………………21 4.3 Enthaply relaxation………………………………………23 五、實驗………………………………………………………………31 5.1 實驗材料……………………………………………………31 5.2 實驗藥品……………………………………………………31 5.3 實驗儀器……………………………………………………32 5.4 實驗步驟……………………………………………………33 5.4.1 樣品製備………………………………………………33 5.4.2 示差掃瞄熱卡計(DSC) ………………………………34 5.4.3 傅立業紅外線光譜儀(FTIR) ………………………35 5.4.4 光學顯微鏡(OM) ……………………………………36 5.4.5 快速傅立葉轉換(FFT) ………………………………37 5.4.6 掃瞄式電子顯微鏡(SEM) ……………………………38 5.4.7 小角度光散射(SALS) ………………………………39 六、結果與討論………………………………………………………42 6.1 混摻物測試…………………………………………………42 6.2 相分離coarsening速率……………………………………45 6.3 Enthalpy relaxation………………………………………65 6.4 sPS/iPS混摻冷結晶…………………………………………97 6.5 sPS/iPS相溶性測試………………………………………112 七、結論………………………………………………………………125 八、參考文獻…………………………………………………………126 九、附錄………………………………………………………………133 十、自述………………………………………………………………136

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