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作者(中文):林士棊
作者(外文):Lin, Shi Chi
論文名稱(中文):開發穿透式電子顯微鏡流體混合式樣品台:應用於臨場觀測含矽嵌段共聚高分子之自組裝行為
論文名稱(外文):Development of Mixing Liquid TEM Holder for In-situ Observing of Self-assembling Co-polymer (PS-b-PDMS)
指導教授(中文):陳福榮
林滄浪
指導教授(外文):Chen, Fu Rong
Lin, Tsang Lang
口試委員(中文):曾繁根
何榮銘
口試委員(外文):Tseng, Fan Gang
Ho, Rong Ming
學位類別:碩士
校院名稱:國立清華大學
系所名稱:工程與系統科學系
學號:103011536
出版年(民國):105
畢業學年度:104
語文別:中文英文
論文頁數:109
中文關鍵詞:穿透式電子顯微鏡流體混合式樣品桿含矽嵌段共聚高分子
外文關鍵詞:Transmission Electron MicroscopyLiquid HolderSelf-assembling Copolymer
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臨場觀測先進技術與封閉及流動式電子顯微鏡的搭配開啟科學界新穎且獨特的領域,本研究以自行設計開發之TEM混合式流體樣品桿 (Mixing Liquid Holder) 並搭配流體晶片 (Flow Cell Chip) 及封閉式SAW Cell作為研究方向,研究成果包括四個部分:
(1) 觀測螢光聚苯乙烯球的混合,進而計算兩種液體的混合比例確認視
野區下的濃度比例。
(2) 觀測碳酸鈣奈米顆粒於石灰水以及小蘇打水液體的注入下而產生可初步確認載具的可用性。
(3) 使用自組裝團塊共聚高分子(PS-b-PDMS)作為觀測樣品,以臨場觀測共聚高分子於氣相溶劑熱退火像轉變之過程。
(4) 開發雙刺激元TEM 樣品載台並使用含矽嵌段共聚高分子進行測試。
本研究展示自製混合流體TEM載具搭配流體晶片不僅成功觀測兩液態化合物混合之化學沈澱反應以及臨場觀測溶劑蒸氣退火應用於含矽嵌段共聚高分子之相轉變過程,以及開發雙刺激元TEM樣品桿,將電子顯微鏡之臨場觀測技術與先進材料研究連結並對重要科學議題做出貢獻。
Advanced techniques with in-situ liquid holder combined with wet cell chips in electron microscopic provide a new territory for us to explore and discover the identifiable scientific issue. The purpose of this research is to develop a mixing liquid holder for TEM with the combination of self-designed flow chips and SAW cells. The results can be shown in four parts.
(1) Observed the mixing process of two different color fluorescent polystyrene beads and then calculate the mixing ratio of the two particles to get the ideal flow rate of the two liquid channels.
(2) Observed the precipitation of calcium carbonate by injecting calcareous water and sodium bicarbonate liquid at the same time to ensure the usable of the mixing liquid holder.
(3) In-situ observing phase transformation of polystyrene-block-polydimethylsiloxane (PS-b-PDMS) treated with toluene solvent vapor annealing process.
(4) Developed heating and liquid holder and applied to PS-b-PDMS.

These results show that self-designed mixing liquid holder with the combination of self-designed flow chips successfully observe the chemical precipitation of calcium carbonate and phase transformation of PS-b-PDMS. This holder is the linking of in-situ observing technique and the advance material research.

Abstract i
摘要 ii
致謝 iii
表目錄 vi
圖目錄 vii
第一章 緒論 1
1.1顯微鏡之發展 1
第二章 文獻回顧 9
2.1初期環境式電子顯微鏡系統 9
2.2微型封閉式環境腔體元件 14
2.3流體交換系統 25
2.4流通式臨場觀測電子顯微鏡系統 27
2.5 共聚高分子溶劑蒸氣退火 34
第三章 實驗方法 40
3.1材料與儀器 40
3.2 Flow chip元件結構及製作方式 49
3.3 微型化濕式腔體元件製成步驟 50
3.4混合式流體穿透式電子顯微鏡樣品桿 52
第四章 結果與討論 54
4.1 混合式流體TEM樣品桿設計與組裝 54
4.2 臨場觀測含矽嵌段共聚高分子(PS-b-PDMS)自組裝現象 76
4.3 臨場觀測含矽嵌段共聚高分子溶劑蒸氣退火過程 82
4.4矽膠氣密系統臨場觀測PS-b-PDMS溶劑蒸氣退火 92
4.5 臨場加熱與流體雙刺激元TEM樣品桿設計 101
第五章 結論 106
第六章 參考文獻 108

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