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研究生:饒全欣
研究生(外文):Chuan-HsinJao
論文名稱:電紡對排聚丙烯及其複合纖維製程與纖維性質分析
論文名稱(外文):Electrospun syndiotactic polypropylene and its composite nanofibers and its property characterization
指導教授:王紀
指導教授(外文):Chi Wang
學位類別:碩士
校院名稱:國立成功大學
系所名稱:化學工程學系碩博士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2012
畢業學年度:100
語文別:中文
論文頁數:124
中文關鍵詞:對排聚丙烯電紡纖維微結構
外文關鍵詞:syndiotactic polypropyleneelectrospinninginternal structure
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本研究以高溫電紡不同濃度對排聚丙烯(sPP)的o-DCB溶液,製備直徑約130-350 nm之sPP纖維。為避免凝膠於電紡製程中形成,先以示差掃描卡計(DSC)測定不同濃度溶液凝膠形成的溫度,再控制電紡油浴溫度為80 oC,使電紡液溫度高於凝膠形成溫度。實驗探討不同含量的鹽類、不同濃度的溶液與以靜態鋁板或快速轉動碟盤收集方式,研究這些變數對電紡纖維的影響。
經由廣角X光繞射(WAXD)、小角X光散射 (SAXS)以及DSC分析電紡纖維微結構。以靜態鋁板收集所得纖維微結構隨溶液濃度不同而有所差異,當濃度低時電紡所得纖維主要為mesophase晶型;當濃度提高時有較多的Form I產生,是因為較高的溶液黏度導致成形纖維中可結晶的分子鏈並未完全結晶,在收集後於室溫下持續結晶成Form I晶體,此現象可由FTIR證實。而快速轉動碟盤收集所得纖維內有較多mesophase存在,這是由於額外的拉伸力所造成。藉由同步輻射光源所得變溫2-D WAXD/SAXS圖譜,可深入探討回火效應對纖維內晶體轉換的影響。在升溫過程中mesophase隨即熔化直到90 oC時完全消失,熔化過程中在較低溫度(35-60 oC)時有Form II晶體的生成,而在較高溫度(60-110 oC)時則生成了Form I晶體。

Syndiotactic polypropylene (sPP) fibers with a diameter of ca. 130-350 nm were successfully produced from high-temperature electrospinning of sPP/o-DCB solutions. To avoid gel formation during process, a jacket-type heat exchanger was used to maintain the solution temperature higher than the gel formation temperature, determined from differential scanning calorimeter (DSC). Several processing factors were investigated to elucidate their effects on the fiber diameter, which included the salt content, the sPP concentration, and the fiber collecting method by using either a stationary plate or a rotating disc.
Through wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS), and DSC analyses, the internal structure of as-spun fibers was characterized. For the sPP fibers collected by a stationary plate, mesophase is the dominant structure and the content of Form I is increased with increasing sPP concentration. The formation of Form I crystal is due to the post-crystallization of the un-crystallizing species at room temperature, which was confirmed by long time FTIR traces. For the sPP fibers collected by a rotating disc, the amount of mesophase was increased since a high stretching force was induced. By the variable-temperature 2-D WAXD/SAXS with synchrotron radiation, the crystal variation of sPP fibers was investigated. On heating, the mesophase starts to melt and disappears completely at 90 oC. Simultaneously, Form II crystal is developed at low temperatures (35-60 oC), followed by the formation of Form I crystal at high temperatures (60-110 oC).

摘要…………………………………………………………………… i
Abstract……………………………………………………… ii
誌謝…………………………………………………………………… iii
目錄…………………………………………………………………… v
表目錄………………………………………………………………… viii
圖目錄………………………………………………………………… ix
符號…………………………………………………………………… xiii
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 聚丙烯簡介…………………………………………………… 5
3.1.1 聚丙烯的介紹…………………………………… 5
3.1.2 對排聚丙烯…………………………… 5
3.2 結晶性sPP之纖維製備與研究……………………… 8
四、 實驗 19
4.1 實驗藥品………………………………………………… 19
4.2 電紡絲儀器及材料……………………………………… 19
4.3 分析儀器………………………………………………… 20
4.4 實驗步驟………………………………………………… 21
4.4.1 電紡絲溶液配製………………………………… 21
4.4.2 電紡絲實驗……………………………………… 21
4.4.3 纖維膜中鹽類的移除………………………… 22
4.4.4 廣角X光繞射儀………………………………… 22
4.4.5 小角X光散射儀………………………………… 23
4.4.6 傅立葉轉換紅外線光譜儀……………………… 24
4.4.7 示差掃描卡計…………………………………… 24
4.4.8 萬能拉力機 ……………………………………… 25
4.5 電紡絲之實驗流程圖…………………………………… 27
五、 結果與討論 28
5.1 溶液性質………………………………………………… 28
5.1.1 溶液配製………………………………………… 28
5.1.2 溶液DSC分析…………………………………… 28
5.2 電紡製程及纖維形態…………………………………… 29
5.2.1 entanglement 濃度, ce…………………………… 29
5.2.2 鹽類添加量之影響……………………………… 29
5.2.3 溶液濃度之影響………………………………… 30
5.2.4 電紡纖維中鹽類的移除………………………… 30
5.2.5 sPP/iPP複合纖維………………………………… 31
5.2.6 sPP/aPP複合纖維………………………………… 31
5.3 sPP纖維微結構分析…………………………………… 32
5.3.1 WAXD分析……………………………………… 32
5.3.2 FTIR分析……………………………………… 35
5.3.3 SAXS分析……………………………………… 36
5.3.4 DSC分析………………………………………… 37
5.4 順向sPP纖維逐步升溫回火過程中晶型轉換………… 38
5.4.1 5A 纖維WAXD分析…………………………… 39
5.4.2 8A 纖維WAXD分析…………………………… 41
5.4.3 5A 纖維SAXS分析…………………………… 42
5.4.4 8A 纖維SAXS分析…………………………… 43
5.4.5 順向纖維WAXD、SAXS結果比較…………… 43
5.5 8A纖維機械性質研究………………………………… 44
5.5.1 最大形變量測試………………………………… 44
5.5.2 固定形變量之往復式拉伸測試……………… 44
5.5.3 非固定形變量之往復式拉伸測試…………… 45
六、 結論…………………………………………………………… 93
七、 參考文獻…………………………………………………… 95
八、 附錄…………………………………………………………… 97

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