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研究生: 曹智翔
Tsao, Chih-Hsiang
論文名稱: 以同步輻射X光散射研究電紡順向纖維升溫時微結構演變
Microstructure evolution of electrospun aligned nanofibers during annealing probed by synchrotron X-ray scattering
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: 2024
畢業學年度: 112
語文別: 中文
論文頁數: 200
中文關鍵詞: 同排聚苯乙烯同排聚丙烯順向纖維小角度X光散射廣角度X光繞射
外文關鍵詞: isotactic polystyrene, isotactic polypropylene, aligned fibers, SAXS, WAXD
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  • 本研究以同步小角/廣角X光散射鑑定電紡所得同排聚苯乙烯(iPS)順向纖維在連續升溫過程中與同排聚丙烯(iPP)順向纖維在逐步升溫過程中,纖維內微結構隨溫度的演變。
    電紡所得iPS順向纖維的結構為amorphous,在溫度高於Tg時,會因為冷結晶而產生晶體。隨著溫度上升,結晶度逐漸增加,但在160 oC以上,增加幅度趨緩。此外,在120 oC下形成的晶體具有高度順向性,隨後在高溫下晶體順向性降低。SAXS分析結果表明,纖維內lamellae的順向性在不同溫度下差異性不大,並且纖維形態在100 oC時有明顯變化,這部分由SEM觀察結果證實。
    電紡所得iPP順向纖維的結構主要為amorphous與mesophase,並夾帶少量a型晶體。隨著溫度上升,原本存在於纖維內的mesophase與少量型晶體逐漸變為只有a型晶體,而amorphous含量並沒有因為mesophase含量減少而增加,顯示iPP順向纖維的冷結晶過程主要是由mesophase轉換為a型晶體所主導。此外,lamellar順向性分析結果顯示,amorphous在高溫下結晶形成的lamellae順向性較高。

    The evolution of the microstructure in aligned isotactic polystyrene (iPS) electrospun fibers during continuous annealing, and aligned isotactic polypropylene (iPP) electrospun fibers during stepwise annealing is characterized by synchrotron small/wide-angle X-ray scattering.
    The dominant structure of aligned iPS as-spun fibers is amorphous. When the annealing temperature (Ta) achieve the glass transition temperature (Tg), relaxation of chains and cold crystallization occur. As Ta increases, the crystallinity gradually increases, but the rate of increase slows down above 160 °C. Moreover, the crystals exhibit high orientation at 120 °C, which decreases at higher Ta. SAXS results indicate that lamellar orientation of remains unchanged at different Ta.
    Aligned iPP as-spun fibers consists mainly of amorphous phase and mesophase components, with a small amount of α-form crystals. As Ta increases, the mesophase and the small amount of α-form crystals initially present in the fibers gradually transform predominantly into α-form crystals, while the amount of amorphous phase does not increase despite the decrease in that of mesophase. This suggests that the cold crystallization process of aligned iPP fibers is primarily dominated by the transformation of the mesophase into α-form. Additionally, lamellar orientation analysis results show that the lamellae formed from the crystallization of the amorphous phase at high Ta exhibit higher orientation.

    摘要 0 Extend abstract ii 誌謝 xii 目錄 xiv 表目錄 xvii 圖目錄 xix 符號表 xxix 一、前言 1 二、簡介 2 2.1 小角度X光散射(SAXS) 2 2.2 廣角度X光繞射(WAXD) 2 三、文獻回顧 3 3.1 同排聚苯乙烯 3 3.2 同排聚丙烯 9 3.3 纖維之X光散射研究 15 四、實驗 33 4.1 實驗材料 33 4.2 實驗儀器 34 4.2.1 iPS順向纖維之X光散射實驗 34 4.2.2 iPP順向纖維之X光散射實驗 34 4.2.3 iPS順向纖維之連續升溫實驗 34 4.3 實驗步驟 35 4.3.1 iPS順向纖維之X光散射實驗 35 4.3.2 iPP順向纖維之X光散射實驗 35 4.4 分析步驟 36 4.4.1 iPS順向纖維之SAXS分析 36 4.4.2 iPP順向纖維之SAXS分析 37 4.4.3 iPS順向纖維之WAXD分析 37 4.4.4 iPP順向纖維之WAXD分析 37 4.4.5 以SEM觀察iPS順向纖維連續升溫時形態演變 38 五、結果與討論 43 5.1 iPS順向纖維連續升溫之WAXD分析 43 5.1.1 2D WAXD圖案與radial繞射強度分布 43 5.1.2 Cake average繞射強度分布與晶體平面間距 45 5.1.3 結晶度計算 46 5.1.4 晶體順向性 47 5.2 iPS順向纖維連續升溫之SAXS分析 48 5.2.1 2D SAXS圖案 48 5.2.2 子午線方向散射強度分布 49 5.2.3 Lamellar特徵長度 52 5.2.4 Lamellar順向度 53 5.2.5 赤道方向散射強度分布 54 5.2.6 使用Ruland方法分析streak散射圖案 54 5.3 以SEM觀察iPS順向纖維連續升溫時形態演變 55 5.4 iPP順向纖維逐步升溫之WAXD分析 55 5.5 iPP順向纖維逐步升溫之SAXS分析 57 5.5.1 2D SAXS圖案 57 5.5.2 子午線方向散射強度分布 58 5.5.3 Lamellar特徵長度 59 5.5.4 Lamellar順向度 60 5.5.5 赤道方向散射強度分布 60 5.5.6 使用Ruland方法分析streak散射圖案 61 六、結論 153 七、參考文獻 154 八、附錄 160

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