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研究生： 謝采娟
Hsieh, Tsai-Chuan
論文名稱： 高溫電紡同排聚丙烯奈米纖維及其微結構鑑定
Preparation of isotactic polypropylene nanofibers via high temperature electrospinning and microstructure characterization
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： 2010
畢業學年度： 98
語文別： 中文
論文頁數： 80
中文關鍵詞： 電紡絲 、聚丙烯 、結晶 、晶型轉換
外文關鍵詞： electrospinning, polypropylene, mesophase, melt-quenched
相關次數： 點閱：127  下載：6 
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    • 可成功由高溫溶液電紡絲法製備出直徑在0.15到1.8m間的同排聚丙烯(iPP)纖維，實驗使用夾套式熱交換器使溶液維持在高溫，並以雷射加熱器加熱針頭至所需溫度。
    由纖維SEM圖可知，當溶液iPP濃度或操作電壓改變時，纖維的形態及直徑分佈也會有明顯的變化，推測是與電紡時溶劑擴散與揮發所需時間有關，將電紡纖維以WAXD做檢測，可知纖維內的晶型為與mesophase的混合晶型。
    經由WAXD、SAXS、FTIR與DSC分析，逐步升溫回火可改變纖維內晶型，同時為了做比較，實驗亦製備了melt-quenched膜並以同樣手法升溫回火，了解其與纖維膜的差異，研究發現升溫回火過程中，amorphous相並不參與分子鏈的重組或晶型的轉換，而由DSC的結果得知，與melt-quenched膜相比纖維膜在分子鏈重組或是晶型轉換，均需較高的溫度，由FTIR的結果可知，晶型轉換時，分子鏈helical的結構皆無改變，SAXS結果顯示了電紡纖維之Bragg spacing皆比melt-quenched膜還要小。

    Isotactic polypropylene (iPP) fibers with diameters between 0.15-1.8 m were successfully produced from high-temperature electrospinning solution using a jacket-type heat exchanger to maintain the solution temperature and a laser heating device to heat locally the needle spinneret to a desired temperature.
    As demonstrated by SEM, there existed a different morphology of iPP fibers by electrospinning of solutions with different concentrations and different voltage. It was related to the solvent evaporation and diffusion during jet whipping. In the as-spun fibers, mixed crystals of the monoclinic a-form and disordered mesophase were detected by WAXD.
    Though wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS), Fourier transform infrared (FTIR) spectroscopy, and differential scanning calorimeter (DSC) analyses, the annealing effect on the structure evolution was investigated. For comparison, step-wise annealing of the melt-quenched film was also carried out. During step-wise annealing, amorphous phase remained unchanged, and the mesophase transformed into  form crystal. DSC results showed that both the reorganization temperature and meso transformation temperature were elevated to higher temperatures compared with those obtained from the melt-quenched film. During the meso transformation, the helical conformation of iPP chains remained intact, as evidenced by FTIR results. At a given annealing temperature, the Bragg spacing derived from SAXS results was smaller in the as-spun fibers than that in the melt-quenched film.

    摘要................................................ i Abstract............................................ ii 致謝................................................ iii 目錄................................................ iv 表目錄............................................... vi 圖目錄.............................................. vii 符號................................................ xi 一、 前言........................................ 1 二、 簡介 2 2.1 電紡絲模式........................... 2 2.2 電紡絲實驗觀察....................... 3 2.2.1 cone和jet形態............... 3 2.2.2 纖維形態.................... 3 三、 文獻回顧 5 3.1 聚丙烯(polypropylene , PP)簡介...... 5 3.1.1 PP的介紹.................... 5 3.1.2 同排聚丙烯(iPP)............. 5 3.2 iPP凝膠(gel)........................ 8 3.3 結晶性高分子之纖維製備與研究........... 8 四、 實驗 33 4.1 實驗藥品............................ 33 4.2 電紡絲儀器及材料..................... 33 4.3 分析儀器............................ 34 4.4 實驗步驟............................ 35 4.4.1 電紡絲溶液配製............... 35 4.4.2 電紡絲實驗................... 36 4.4.3 纖維膜中鹽類的去除............ 36 4.4.4 melt-quenched膜的製備........ 36 4.4.5 廣角度X光繞射儀 (WAXD) ....... 37 4.4.6 小角度X光散射儀 (SAXS) ....... 37 4.4.7 傅立葉紅外線光譜儀 (FTIR ) ... 37 4.4.8 示差掃描卡計 (DSC) .......... 38 4.5 電紡絲之實驗流程圖.................... 40 五、 結果與討論 41 5.1 溶液性質............................. 41 5.1.1 溶液配製..................... 41 5.1.2 溶液之DSC分析................ 41 5.2 操作電壓對纖維及製程的影響.............. 42 5.2.1 entanglement 濃度, ce........ 42 5.2.2 電紡製程之影響................ 42 5.2.3 纖維及結晶形態................ 43 5.3 iPP纖維之分析......................... 44 5.3.1 不同濃度之纖維形態............. 44 5.3.2 纖維結晶型態.................. 45 5.3.3 纖維DSC分析.................. 45 5.4 iPP纖維在升溫回火時的晶型轉換........... 46 5.4.1 WAXD........................ 46 5.4.2 SAXS......................... 47 5.4.3 FTIR......................... 49 六、 結論.......................................... 78 七、 參考文獻...................................... 79

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