新穎質子交換膜

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吳千舜(Chien-Shun Wu) 查詢紙本館藏

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化學學系

論文名稱

新穎質子交換膜
(Novel Proton Exchange Membrane)

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摘要(中)

直接甲醇燃料電池的質子交換膜主要研究焦點集中於限制薄膜在甲醇水溶液下的過度膨潤，降低甲醇滲透現象(Crossover)並同時維持薄膜的高導電度。本研究利用原位(in-situ)聚合的方式，在PVDF/HFP (Poly (vinylidenefluoride-co-hexafluoropropylene)共聚高分子溶液中做磺酸酚醛的聚合反應並製備成質子交換膜。在此，磺酸酚醛會在高分子表面形成一親水性披覆膜而呈現反微胞(inverse micelle)的型態，且鄰近的磺酸根是暴露於PVDF/HFP球體間所形成的質子滲透通道並且是互相排列整齊，這樣所形成的離子導電機制將會不同於先前其他系統所研究。更進一步，對於在高濃度甲醇水溶液中，因為PVDF/HFP高分子本身具有部分的結晶性，所以會抑制薄膜的過度膨潤而且可保持質子滲透通道的尺寸安定性，進而有效降低薄膜的甲醇滲透現象。本研究的最後將薄膜再做進一步的交聯，使薄膜應用於直接甲醇燃料電池時更具有較高的化學及熱穩定性。

摘要(英)

Conventional membranes such as Nafion suffer from the swelling and methanol crossover under high methanol concentration fuel stream. More durable proton exchange membrane (PEM) has received increasing interests from academic and industrial research for direct methanol fuel cell (DMFC) application. However, most efforts to reduce crossover effect is achieved by discriminating water and methanol permeation, usually at the cost of the proton conductivity. This dilemma is resolved by taking advantage of the novel conducting mechanism, which occurs in nano-ionics: membranes with and channels decorated with closely spaced sulfonic groups in connected nano-pores. Here proton transfer is established by the directional tunneling through the surface charge field created by finely dispersed nano flow channel. Previous studies have demonstrated that polymerization of phenolic in the PVdF and PVdF-HFP copolymers solution forms a thin crust of hydrophilic shell on the sol surface. Current study expands such design using inverse micelle formation where the sulfonic groups are exposed and extend in the solvent permeation channel (with dimensions less than 20 nm). The closely spaced arrangements establish a novel proton conducting behavior entirely different from those previously observed in other systems. As a result of the nano-flow structure, crossover is effectively reduced. Since the PVdF-HFP substrate is partially crystallized, the film withstands solvent swell and preserved the membrane dimensions even in high methanol concentration. Further cross-linking of the product leads to highly chemical and thermally stable membrane suitable for the application of direct methanol fuel cell (DMFC) .

關鍵字(中)

★ 直接甲醇燃料電池
★ 質子交換膜
★ 甲醇滲透現象
★ 原位聚合
★ 反微胞型態

關鍵字(英)

★ nano-ionics
★ Direct methanol fuel cell (DMFC)
★ Proton exchange membrane (PEM)
★ inverse micelle

論文目次

目錄頁次
中文摘要………………………………………………………………..Ⅰ
英文摘要………………………………………………………………..Ⅱ
目錄……………………………………………………………………..IV
表目錄……………………………………………………………….…VII
圖目錄……………………………………………...…………………VIII
第一章緒論……………………………………………………………1
1-1 前言……………………………………………………………...1
1-2 研究動機………………………………………………………...4
第二章文獻回顧………………………………………………………7
2-1 質子交換膜的種類……………………...………………………8
2-1-1 離子聚合物薄膜………………………………………9
2-1-2有機/無機混成薄膜…………………………………….23
2-1-3酸/鹼高分子薄膜……………………………………….29
第三章實驗技術及原理……………………………………………..33
3-1 樣品製備…………………………………………………….…33
3-1-1 聚合型(in situ)質子交換膜之製備………………….…..33
3-1-2 交聯型(in situ)質子交換膜之製備………………….…..33
3-1-3 實驗藥品……………………………………………….34
3-2 微差掃瞄熱卡計(Differential Scanning Calorimeter，DSC)…35
3-2-1 DSC實驗操作程序..………………………………….. 36
3-3 熱重量分析儀(Thermo gravimetric analyzer，TGA )……..….36
3-3-1 TGA實驗操作程序…………………………………….36
3-4 傅立葉式紅外線吸收光譜儀(FT-IR)…………………………37
3-4-1 FT-IR實驗操作程序…………………………………...38
3-5 掃瞄式電子顯微鏡（Scanning Electron Microscopy，SEM）….38
3-5-1 SEM實驗操作程序…………………………………….39
3-6 X光射線繞射(X-Ray diffraction)……………………………..39
3-6-1 X光射線繞射實驗操作程序…………………….…….40
3-7 交流阻抗分析儀(AC Impedance)……………………………..40
3-7-1 導電度兩種量測方法………………………………….41
3-7-2 等效電路(equivalent circuit)…………………………...48
3-7-3 AC-impedance實驗操作程序…………………………51
3-8 固態核磁共振儀（Solid state NMR） …………………………52
3-9 吸水膨潤比(solvent uptake) …………..………………………52
3-10 離子交換容量 (Ion Exchange Capacity;IEC)………………...52
3-10-1 離子交換容量實驗操作程序………………………...53
第四章結果與討論………………………………………...………...54
4-1 13C固態核磁共振(13C Solid State NMR) ……...……………...56
4-2 傅立葉紅外線光譜 ( FT-IR )分析……...……………………..59
4-3 微差掃瞄熱卡計(DSC)分析……...…………………………...65
4-4 X光粉末繞射儀(XRD)分析……...…………………………...73
4-5 熱重量分析儀（TGA）……………………………………….79
4-6 SEM分析…………………………………………………..…..81
4-7 吸水與吸甲醇膨潤比(Solvent uptake)…….……….……..…..87
4-8 交流阻抗儀(AC impedance)分析…….……….…………..…..92
第五章結論………..…………………………………………….…96
第六章參考文獻……………………………………………………98
表目錄
表1-1 燃料電池的種類………………………..………………………2
表1-2 電池能量密度之比較......................................3
表2-1 商業化的質子交換膜………….……………………………...11
表2-2 修飾PFSA的薄膜一覽表…………………………………….16
表2-3 有機-無機複合膜一覽表…………………...…………………26
表2-4 氫氧燃料電池和直接甲醇燃料電池在高溫測試下的結果....31
表3-1 本研究所使用的藥品及其代號，結構…….…………………34
表3-2 Impedance equations for Equivalent circuit Elements………...48
表4-1 PVDF-HFP/磺酸酚醛交聯前後之DSC分析數據(第二次掃瞄)………….72
表4-2 不同比例的PVDF-HFP/磺酸酚醛薄膜之導電度與IEC值…….…………93
表4-3 HMTA交聯的PVDF-HFP/磺酸酚醛薄膜之導電度與IEC值………………95
表4-4 Epoxy交聯的PVDF-HFP/磺酸酚醛薄膜之導電度與IEC值…………………95
表4-5 DMF和NMP溶劑所製備出來薄膜的導電度………………95
圖目錄
圖1-1 PEM燃料電池……………………………………………….....2
圖1-2 質子交換膜的反微胞形式設計概念………………………......6
圖1-3 交聯型的質子交換膜………………………………………..…6
圖2-1 離子聚合物的微結構…………………………...……………...9
圖2-2 質子傳導機制………………………………………………....10
圖2-3 薄型的PFSA強化膜…………………………………………..13
圖2-4 Nafion和碳氫高分子之微結構……………..……………...19
圖2-5 溶膠-凝膠法製備有機-無機混成膜………………………..25
圖3-1 四點探針法的測量裝置圖……………………………………42
圖3-2 Nyquist diagram of AC impedance……………………………44
圖3-3 阻抗函數Z在複數平面上之表示圖…………………………45
圖3-4 簡單電子元件及其組合之交流阻抗圖譜：(a)單一電阻；(b)
單一電容；(c)；電阻與電容串聯；(d)電阻與電容並聯…..47
圖3-5 Equivalent circuit I of an electrochemical cell………..……….49
圖3-6 Equivalent circuitⅡof an electrochemical cell……………...…50
圖3-7 Equivalent circuit Ⅲof an electrochemical cell……………….50
圖3-8 AC Impedance 裝置圖……………………………………..…51
圖4-1 論文研究架構之流程圖……………………………………55
圖4-2 PVDF-HFP/磺酸酚醛交聯前後的13C-NMR光譜圖(a)PH20%SP ; (b)PH50%SP ;
(c)PH18%SP10%HMTA (d)PH45%SP10%HMTA; (e)PH45%SP10%Epoxy; (f)PH18%SP10%
Epoxy……………………………………….58
圖4-3 純PVDF-HFP和磺酸酚醛的IR分析光譜圖……………........................…60
圖4-4 不同比例的PVDF-HFP/磺酸酚醛之IR分析光譜圖：(a)PVDF-HFP (b)PH20SP
(c)PH50SP (d)PH60SP (e)PH70SP (f)SP………………………….......…………63
圖4-5 HMTA交聯的PVDF-HFP/磺酸酚醛之IR分析光譜圖：(a)PVDF-HFP (b)PH18SP10H
(c)PH45SP10H (d)PH54SP10H (e)PH63SP10H (f)SP……………………........…64
圖4-6 Epoxy交聯的PVDF-HFP/磺酸酚醛之IR分析光譜圖：(a)PVDF-HFP (b)PH18SP10E
(c)PH45SP10E (d)PH54SP10E (e)PH63SP10E (f)SP………….……….....………65
圖4-7 不同比例的PVDF-HFP/磺酸酚醛之DSC分析圖……..…….68
圖4-8 HMTA交聯的PVDF-HFP/磺酸酚醛之DSC分析圖……….70
圖4-9 Epoxy交聯的PVDF-HFP/磺酸酚醛之DSC分析圖…….….71
圖4-10 (a)PVDF-HFP粉末 (b)以DMF為溶劑鑄成的PVDF-HFP薄膜之XRD分析圖……………74
圖4-11 不同比例的PVDF-HFP/磺酸酚醛薄膜之XRD分析圖……..74
圖4-12 HMTA交聯的PVDF-HFP/磺酸酚醛之XRD分析圖.........75
圖4-13 Epoxy交聯的PVDF-HFP/磺酸酚醛之XRD分析圖……..76
圖4-14 Nafion 117浸泡在水及甲醇溶液後之XRD分析圖…….…77
圖4-15 PH60SP浸泡在水及甲醇溶液後之XRD分析圖………..…77
圖4-16 PH54SP10H浸泡在水及甲醇溶液後之XRD分析圖………78
圖4-17 PVDF-HFP/磺酸酚醛之TGA分析圖……………………....80
圖4-18 PVDF-HFP/磺酸酚醛之DTG分析圖…………………….…80
圖4-19 PVDF/HFP高分子薄膜之SEM分析： (a) ×100；(b) ×500；(c) ×1.0k；
(d) ×2.0k……………….……..…….82
圖4-20 不同比例的PVDF-HFP/磺酸酚醛薄膜之SEM分析：PH20SP：(a) ×1.0k (b) ×2.0k；
PH50SP：(c) ×1.0k(d) ×2.0k………………………………………83
圖4-21 HMTA交聯的PVDF-HFP/磺酸酚醛薄膜之SEM分析：PH18SP10H：(a) ×1.0k
(b) ×2.0k；PH45SP10H：(c) ×1.0k (d) ×2.0k……………………………..……85
圖4-22 Epoxy交聯的PVDF-HFP/磺酸酚醛薄膜之SEM分析：PH18SP10E：(a) ×2.0k
(b) ×5.0k；PH45SP10E：(c)×2.0k (d) ×5.0k ; PH63SP10E：(e) ×1.0k
(f) ×2.0k……………..............................................…86
圖4-23 商業化質子交換膜Nafion 117的吸水與吸甲醇膨潤比…..87
圖4-24 PVDF-HFP/磺酸酚醛薄膜的吸水膨潤比值……….…….…89
圖4-25 HMTA交聯的PVDF-HFP/磺酸酚醛薄膜的吸水膨潤比值….................…90
圖4-26 Epoxy交聯的PVDF-HFP/磺酸酚醛薄膜的吸水膨潤比值…………………………90
圖4-27 DMF和NMP溶劑所製備出來薄膜的吸水與吸甲醇膨潤比……………………………91
圖4-28 PH60SP薄膜在不同甲醇濃度水溶液下所測得的離子導電度及溶劑吸附量………93

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指導教授

諸柏仁(Po-Jen Chu)

審核日期

2004-7-19

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