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研究生: 林健樺
Lin, Jian-Hua
論文名稱: 以電紡絲製備聚苯乙烯纖維膜
Preparation of polystyrene-fiber membranes via electrospinning
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: 2004
畢業學年度: 92
語文別: 中文
論文頁數: 198
中文關鍵詞: 高速攝影機電紡絲聚苯乙烯纖維雙折射率差圓錐液柱甩動
外文關鍵詞: polystyrene fiber, birefringence, jet, high-speed photographs, splaying, electrospinning
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  •   以電紡絲製備極細纖維,在低沸點或易與水氣混合之溶劑於系統裡,常會導致Taylor cone在形成前(或之後)即生成阻塞物於針端,使過程停止。本實驗則藉由飽和的溶劑蒸氣或氮氣導引至針端來改善阻塞的問體,使過程能連續運作。

      纖維直徑和雙折射率的變化會因為溶液黏度、導電度、流量及工作距離而影響。在這些變數裡,以溶液導電度的影響最大。

      在電紡絲的過程裡,溶液在低濃度和高導電度時,針端形成的圓錐會接近半圓球狀,液柱被侷限在圓錐的尖端噴出。在這條件下,能製備出極細的纖維。在這些變數裡,流量改變對液柱的長度影響最小,製備的纖維膜直徑最主要受到工作距離的改變而影響,而工作距離對液柱直徑則影響最小。

      藉由高速攝影機的拍攝,可以觀察到dripping、pulsating和splaying的過程。溶液在低濃度時,在splaying過程裡會觀察到有很多珠狀於甩動的液柱裡。

      以DMF為溶劑之系統裡,溶液濃度為5wt%,TEBAC鹽含量為1wt%時,製備出平均直徑在112 30nm的聚苯乙烯纖維。以THF為溶劑之系統裡,溶液濃度為7wt%,LiClO4鹽含量為1wt%時,製備出平均直徑在95 51nm的聚苯乙烯纖維。以chloroform為溶劑之系統裡,溶液濃度為7wt%,Bu4NClO4鹽含量為1wt%時,製備出平均直徑在297 77nm的聚苯乙烯纖維。

      Over the last few years the electrospinning of thin fiber has been the subject of many investigations. In systems where the solvent used has a low boiling point or miscible with the moisture, the droplet at the tip become blocked very quickly during, (or before,) the formation of the Taylor cone, making the process discontinuous. In this experiment, a special design is used to confine the needle tip in the atmosphere with a saturated solvent or a nitrogen gas.

      The fiber diameter and birefringence depend on the parameters such as solution viscosity, conductivity, solution feeding rate and working distance. The conductivity was found to have a more significant effect on the fiber diameter and birefringence than the other parameters.

      For solution with relatively low concentration and high conductivity, the jet formation zone is limited to the apex of the meniscus. These conditions make it possible to obtain very fine fibers. Feeding rate was found to have no effect on the jet length than the other parameters. The varying working distances only affect the diameter of electrospun area.

      High-speed photographs showed the process of dripping, pulsating or splaying. For solution with low concentration, small beads were viewed in a whipping liquid jet.

      The average diameter of electrospun fibers was 112 30nm from a 5wt% solution of polystyrene in DMF with 1wt% TEBAC.

      The average diameter of electrospun fibers was 95 51nm from a 7wt% solution of polystyrene in THF with 1wt% LiClO4.

      The average diameter of electrospun fibers was 297 77nm from a 7wt% solution of polystyrene in chloroform with 1wt% LiClO4.

    中文摘要 i 英文摘要 ii 致謝 iv 目錄 v 表目錄 viii 圖目錄 ix 符號 xv 一、前言 1 二、簡介 2 2.1電紡絲之模式 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電紡絲實驗之流程 3 2.2.1 Cone和Jet之形態 4 2.2.2 Jet甩動之過程 4 2.2.3纖維膜之面積 4 2.2.4纖維之形態 4 三、文獻回顧 16 3.1電紡絲之過程 16 3.2影響電紡絲之因子 17 3.3纖維的排列 19 3.4奈米化之聚苯乙烯纖維 20 四、理論 48 4.1 繞射理論 48 4.1.1單狹縫或長方形孔洞 48 4.1.2圓形孔洞 50 4.2 雙折射原理 51 五、實驗 59 5.1 實驗藥品 59 5.2 實驗材料及儀器 60 5.2.1量測溶液性質之儀器 60 5.2.2常溫及高溫電紡絲儀器及材料 61 5.2.3光學儀器 63 5.3 實驗步驟 65 5.3.1 溶液製備 65 5.3.1.1 亂排聚苯乙烯溶液 65 5.3.1.2 對排聚苯乙烯溶液 65 5.3.2儀器操作步驟 66 5.3.2.1 雷射量測液柱直徑 66 5.3.2.2 高速攝影機觀察纖維成形 68 5.3.2.3 氮氣流量校正 69 5.3.2.4 纖維雙折射率量測 69 5.3.3室溫電紡絲實驗 71 5.3.3.1無氮氣裝置 71 5.3.3.1有氮氣裝置 71 5.3.4高溫電紡絲實驗 71 六、結果與討論 78 6.1亂排聚苯乙烯纖維之製備 83 6.1.1 以DMF為溶劑之系統 83 6.1.1.1針端阻塞之現象 83 6.1.1.2操作電壓的量測 85 6.1.1.3不同因子對纖維直徑及雙折射率之影響 86 6.1.1.4電紡絲過程之觀察 88 6.1.1.5微奈米化之聚苯乙烯纖維 90 6.1.2以THF為溶劑之系統 91 6.1.2.1針端阻塞之現象 91 6.1.2.2以co-solvent之方法改善針端阻塞之問題 91 6.1.2.3以導引THF蒸氣至針端之方法改善針端阻塞之問題 91 6.1.3以chloroform為溶劑之系統 92 6.1.3.1針端阻塞之現象 92 6.1.3.2以導引chloroform蒸氣至針端之方法改善針端阻塞之問題 92 6.2以高速攝影機觀察結果 171 6.2.1 Dripping mode 171 6.2.2 Pulsating mode 171 6.2.3 Splaying region 171 6.3 對排聚苯乙烯纖維之製備 179 七、結論 182 八、參考文獻 185 附錄 192 自述 198

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