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研究生: 高淑雅
Kao, Shu-Ya
論文名稱: 高溫電紡聚乙烯奈米纖維及其微結構鑑定
Preparation of polyethylene 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: 160
中文關鍵詞: 高溫電紡絲LLDPEmPEUHMWPE
外文關鍵詞: high-temperature electrospinning, LLDPE, mPE, UHMWPE
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  • 本實驗利用高溫電紡設備製備PE奈米纖維,並研究不同PE(LLDPE、mPE、UHMWPE)與鹽類濃度對電紡所得纖維的影響。成形纖維分析鑒定使用 DSC、FTIR、WAXD與SAXS瞭解製程的改變對纖維微結構的影響,實驗發現:添加高濃度鹽於電紡液,能有效提高導電度,使液柱在電紡過程中劇烈拉伸,形成直徑較細的纖維,使用超高分子量的UHMWPE,與其他兩種PE相較,可在較低濃度時形成entangled溶液,而藉由纖維直徑與溶液濃度成反比的關係,達到獲得奈米級纖維的目的。
    在UHMWPE纖維內分子鏈受拉伸,排列情形較整齊,DSC升溫過程會有高熔點;由FTIR與WAXD結果觀察到含有少量的半穩定monoclinic晶型,研究發現逐步升溫回火過程monoclinic晶型會在65度時轉換為orthorhombic,並有冷結晶情形的出現,結晶度持續上升後於120度開始下降。
    LLDPE溶液中添加mPE可形成混摻溶液,對電紡製程不會造成太大影響,但纖維直徑變小且結晶度下降。

    This research was to prepare PE nano-fibers by high-temperature solution electrospinning, and to study the effects of material(LLDPE, mPE, UHMWPE) and concentration of salts on the as-spun fibers. Solutions with high conductivity by adding more salts allowed significant elongation during electrospinning, and thinner fibers would be collected. Ultra high molecular weight PE(UHMWPE) was better than the other two PEs to become entangled solution easily, and nano-fibers could be readily obtained from dilute solutions.
    For comparison, casting film was also prepared for analysis. Polymer chains in UHMWPE fibers were more ordered than those in the casting film, and a high melting point was observed from DSC heating traces. In the as-spun fibers, few crystals of meta-stable monoclinic form were detected by FTIR and WAXD. During step-wise annealing, the monoclinic crystals transformed into the orthorhombic crystals, and crystallinity was also increased.
    When LLDPE solution was blended with mPE, there was no effect on electrospinning process, but fiber diameter was reduced and the fiber crystallinity was decreased.

    摘要-i Abstract-ii 致謝-iii 目錄-iv 表目錄-viii 圖目錄-x 一、前言-1 二、簡介 2.1 電紡絲模式-2 2.1.1 dripping mode-2 2.1.2 pulsating mode-2 2.1.3 cone-jet mode-3 2.1.4 multi-jet mode-3 2.2 電紡絲實驗觀察-3 2.2.1 cone和jet形態-3 2.2.2 jet甩動過程-3 2.2.3 纖維形態-4 三、文獻回顧 3.1 聚乙烯簡介-7 3.1.1 超高分子量聚乙烯(UHMWPE)-8 3.1.2 線性低密度聚乙烯(LLDPE)-9 3.1.3 metallocene聚乙烯(mPE)-9 3.2 聚乙烯紡絲簡介-10 3.3 高溫電紡絲簡介-11 3.4 聚乙烯性質-12 四、實驗 4.1 實驗材料與藥品-27 4.2 實驗儀器-27 4.2.1 電紡絲製備儀器-27 4.2.2 檢測儀器-30 4.3 樣品製備-31 4.3.1 電紡溶液製備-31 4.3.2 電紡纖維製備-31 4.3.3 電紡纖維去除鹽類-32 4.3.4 熱壓試片製備-32 4.3.5 casting試片製備-33 4.4 實驗步驟-33 4.4.1 導電度量測-33 4.4.2 示差掃描卡計(DSC)-33 4.4.3 傅立葉轉換紅外線光譜(FTIR)-35 4.4.4 廣角度X光繞射(WAXD)-36 4.4.5 小角度X光散射(SAXS)-36 4.4.6 偏光顯微鏡(POM)-36 4.4.7 掃描式電子顯微鏡(SEM)-36 4.4.8 穿透式電子顯微鏡(TEM)-37 4.4.9 電紡實驗流程圖-38 五、結果與討論 5.1 電紡溶劑與鹽類的選擇-39 5.1.1 溶劑的選擇-39 5.1.2 鹽類的選擇-39 5.2 電紡溶液性質-41 5.2.1 LLDPE-41 5.2.2 mPE-42 5.2.3 LLDPE/mPE混摻-42 5.2.4 UHMWPE-43 5.3 電紡絲實驗分析-44 5.3.1 LLDPE-44 5.3.2 mPE-46 5.3.3 LLDPE/mPE混摻-47 5.3.4 UHMWPE-48 5.4 纖維形態-50 5.4.1 LLDPE-50 5.4.2 mPE-51 5.4.3 LLDPE/mPE混摻-52 5.4.4 UHMWPE-52 5.5 纖維熱分析-54 5.5.1 LLDPE-54 5.5.2 mPE-55 5.5.3 LLDPE/mPE混摻-56 5.5.4 UHMWPE-57 5.6 纖維結晶形態-57 5.6.1 LLDPE-57 5.6.1.1 FTIR-58 5.6.1.2 WAXD-58 5.6.1.3 SAXS-59 5.6.2 mPE-60 5.6.2.1 FTIR-60 5.6.2.2 WAXD-60 5.6.3 LLDPE/mPE混摻-60 5.6.3.1 FTIR60 5.6.3.2 WAXD-61 5.7 電紡纖維內鹽類的去除-61 5.7.1 鹽類去除方法探討-62 5.7.2 浸泡oDCB對纖維形態的影響-62 5.7.3 電紡纖維元素分析-63 5.7.4 電紡纖維結晶形態分析-64 5.7.4.1 熱分析-64 5.7.4.2 FTIR-64 5.7.4.3 WAXD-65 5.8 UHMWPE電紡纖維升溫過程結晶形態分析-66 5.8.1 FTIR-66 5.8.2 WAXD-67 5.8.3 SAXS-68 六、結論-140 七、參考文獻-141

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