利用小角度X光散射和廣角度X光繞射探討聚環氧乙烷於醇類中的結晶現象

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胡婉瑜(Wan-Yu Hu) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

利用小角度X光散射和廣角度X光繞射探討聚環氧乙烷於醇類中的結晶現象

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至系統瀏覽論文 (2026-7-24以後開放)

摘要(中)

聚環氧乙烷 (Poly(ethylene oxide), PEO) 因其材料特性和複雜的相行為成為高分子科學中有趣的研究領域之一。本研究實驗結果表明，PEO在熔點以上完全溶解於不同種類的醇（甲醇、乙醇、異丙醇和丁醇）中。然而，將樣品靜置於室溫數分鐘至數天，或是將其進行冰浴，會發現其從原本的溶液態轉變形成不透明的凝膠狀混合物，而這樣的凝膠狀結構是具有熱可逆性的。為了研究溶液-凝膠的轉變，使用了掃描式微分熱卡計 (Differential scanning calorimetry , DSC)來進行熱行為之測定，其量測結果表明，所觀察到溶液因溫度變化而產生凝膠化的現象，與其結晶行為密切相關。利用小角度X光散射 (SAXS)和廣角度 X光繞射 (WAXS) 進行量測，並結合模型的擬合，證明了溶液-凝膠的轉變和PEO結晶行為之間的相關性。研究結果表明，PEO 在高溫下完全溶解並均勻分散在溶液中，當冷卻溫度低於臨界溫度後，PEO的結晶會以層狀堆疊的方式形成，凝膠由三維的網狀結構構成。

摘要(英)

Poly(ethylene oxide) (PEO) is one of the most intriguing research field in macromolecular science due to materials properties and complex behavior. The results demonstrated that PEO is completely dissolved in different kinds of alcohols (methyl alcohol, ethyl alcohol, isopropyl alcohol, and butyl alcohol) above crystal-melting points. However, after quenching the mixtures to room temperature, the solutions form an opaque gel-like mixture. The gel-like structure is thermally reversible. To investigate sol-gel transitions, differential scanning calorimetry (DSC) was used. DSC curves show that the gelation behavior in PEO solutions could occur and correlate with crystalline morphology. Correlations between the phase separation behavior and crystalline morphology was investigated through in-situ small-angle X-rays scattering (SAXS), wide-angle X-rays scattering (WAXS), and model fitting. The study shows that PEO is completely well dissolved in the solution at high temperature. After cooling down to a critical temperature, PEO crystallizes into a three-dimensional network of lamellar stacks. The 3D network results in a hard gel for PEO in ethanol, propanol and butanol.

關鍵字(中)

★ 均聚物
★ 結晶
★ 凝膠

關鍵字(英)

論文目次

目錄

摘要 i
Abstract ii
致謝 iii
目錄 iv
圖目錄 vi
表目錄 x
第1章簡介 1
1-1 均聚物與嵌段共聚物 1
1-2 聚環氧己烷(PEO)的應用 2
1-2-1 碳捕獲共聚物薄膜 2
1-2-2 鋰電池黏合劑(binder) 4
1-2-3 高分子固態電解質(polymer electrolyte) 6
1-3 凝膠 8
1-3-1 凝膠的分類 9
1-3-2 凝膠的結構與其形成的機制 9
1-4 影響凝膠形成之因子 14
1-4-1 pH值 14
1-4-2 溫度 16
1-4-3 溶劑 19
1-4-4 添加鹽離子 20
1-5 研究動機 21
第2章實驗 22
2-1 實驗藥品 22
2-1-1 實驗藥品 22
2-2 實驗樣品製備 24
2-3 實驗儀器 25
2-3-1 掃描式微分熱卡計(Differential scanning calorimetry, DSC) 25
2-3-2 小角度X 光散射（Small Angle X-ray Scattering, SAXS）和廣角度X光散射(Wide Angle X-ray Scattering, WAXS) 26
2-4 擬合軟體(SasView) 29
2-4-1 Unified exponential/Power-law (Beaucage model)模型 30
2-4-2 Two Lorentzian model模型 31
2-4-3 lamellar stack paracrystal模型 33
第3章結果與討論 35
3-1 均聚物在溶劑中的自組裝行為 35
3-2 溫度效應對凝膠之影響 37
3-2-1 聚環氧乙二醇之熱行為探討 39
3-3 臨場(in-situ)實驗之結構探討 46
3-3-1 降溫臨場實驗之結構變化 47
3-3-2 持溫臨場實驗之結構變化 55
3-3-3 升溫臨場實驗之結構變化 64
3-3-4 結構變化之溫度探討 68
第4章結論 70
第5章參考文獻 71
第6章附錄 78

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指導教授

黃俊仁孫亞賢(Chun-Jen Huang Ya-Sen Sun)

審核日期

2023-7-27

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