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研究生： 高鴻哲
Hung-Che Kao
論文名稱： 4,4’-氧雙鄰苯二甲酸酐及環氧樹脂交聯磺酸化聚乙烯醇用於質子交換膜燃料電池之研究
Cross-linked of 4,4’-Oxydiphthalic anhydride and Epoxy Incorporating Sulfonated Poly (vinyl alcohol) for PEMFC Applications
指導教授： 蕭敬業
Ching-Yeh Shiau
口試委員: 黃炳照
Bing-Joe Hwang
林智汶
Chi-Wen Lin
學位類別： 碩士
Master
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2010
畢業學年度： 98
語文別： 中文
論文頁數： 150
中文關鍵詞： 4-4'-氧雙鄰苯二甲酸酐 、磺酸化 、交聯反應 、4-醛基-1-3苯磺酸鈉鹽 、聚乙烯醇 、質子交換膜燃料電池 、環氧樹脂
外文關鍵詞： Sulfonated, ODPA, Epoxy, PEMFC, Cross-linked, DSDSBA, PVA
相關次數： 點閱：378  下載：4 
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    • 本研究著重於發展質子交換膜燃料電池（Proton exchange membrane fuel cell，簡稱 PEMFC）之電解質薄膜，以取代價格昂貴且甲醇滲透率過高的Nafion薄膜，選擇良好成膜性、化學穩定性佳及價格便宜之聚乙烯醇（Poly(vinyl alcohol)，簡稱PVA）作為質子交換膜主體，利用二甲基亞（Dimethylsulfoxid，簡稱DMSO）當作溶劑，再利用4-醛基-1,3苯磺酸鈉鹽（4-Formyl-1,3-Benzenedi-sulfonic acid,disodium salt，簡稱DSDSBA）作磺酸化（Sulfonation）處理得到帶有磺酸鈉鹽的聚乙烯醇（SPVA），導入不同比例之4,4'-氧雙鄰苯二甲酸酐（4,4'-Oxydiphthalic anhydride，簡稱ODPA）及環氧樹脂（Epoxy）合成為一交聯結構。本研究主題為探討其交聯SPVA之物理性質、熱性質及電化學性質分析。
    從FTIR圖譜得知，PVA上的OH－基團與DSDSBA上之aldehyde基會透過羥醛反應，而改質成帶有磺酸鈉鹽的聚乙烯醇狀態。從TEM圖結果得知，在低交聯程度之質子交換膜（SOE3）中，其展現較均相的離子叢聚分散於高分子基材中。由於較均相的離子叢聚，縮短質子傳遞的距離，有利質子傳導，進而提升其導電度，在20 ℃下導電度可達2.70 × 10-2 S/cm，持續升溫至70 ℃，導電度可達0.208 S/cm；相較於高交聯程度之交換膜（SOE50），因（親疏水相）相分離居多，導致質子傳遞距離變長，導電度於20 ℃下只有2.46 × 10-3 S/cm的表現。
    磺酸化程度隨著交聯劑添加量減少，而磺化比例相對增加，IEC值可達1.69 mmole/g。因SOE3薄膜IEC值高，在室溫下的含水率可達133.07 wt %。於電池測試分析中，導電度最佳的SOE3薄膜卻不如表現，在濕式氫氣與氧氣電池性能中於70 ℃下，功率密度只有154 mW/cm2的表現，交聯程度持續增加，薄膜（SOE7）功率密度可達443 mW/cm2。

    The aim of this study is to develop a new polymer electrolyte membrane for low temperature proton exchange membrane fuel cells (PEMFCs), which is taken as a possible alternative to the state-of-the-art Nafion membrane having drawbacks such as high cost and high methanol crossover. The low cost, easy film-fabrication and good chemical stability of poly(vinyl alcohol) (PVA) is chosen as the matrix backbone of proton exchange membranes. Dimethylsulfoxid (DMSO) is the cross-linked agent for the reaction.
    In addition, 4-Formyl-1,3-Benzenedisulfonic acid disodium salt (DSDSBA) is employed as the sulfonated agent to increase the sulfonic acid groups of PVA. The degree of sulfonation for PVA is controlled with different ratios of 4,4'-oxygen double-phthalic anhydride (4,4'-Oxydiphthalic anhydride, referred to as ODPA) and epoxy resin (Epoxy), and the whole cross-linked-type structure is therefore formed. The corresponding physical and thermal properties are characterized and correlated with its electrochemical properties.
    First of all the FTIR spectra provide the evidence for the condensation reaction between hydroxyl groups and aldehyde groups. The TEM images of the prepared membrane indicate better homogeneous dispersion of ion clusters in the polymer matrix for low-degree cross-linked proton exchange membrane (SOE3), which implies a shorter distance in between the ionic clusters. Nevertheless the proton transfer between ionic clusters becomes easier, resulting in an improvement of the bulk ionic conductivity. (2.70 × 10-2 S cm-1@ 20 oC and 0.208 S cm-1@ 70 oC. For high-degree cross-linked exchange membrane (SOE50), hydrophobic/hydrophilic phase separation results in the increase of the proton transfer distance. The ionic conductivity is therefore reduced (2.46 × 10-3 S cm-1@ 20 oC).
    The degree of sulfonation of cross-linked structure increases with reducing cross-linked agent. The highest IEC value is up to 1.69 mmole g-1(SOE3) with water content up to 133.07 wt% at room temperature. However the ionic conductivity of the SOE3 membrane is not as good as the prediction, which may be due to the low degree of cross-linked, which the structure was destroyed during activation and only delivers a peak power density of 154 mW cm-2 with wet H2/O2 at 70 oC. The proposed reason can be evidenced by the performance of the membrane (SOE7) of higher degree of cross-linked, which the peak power density can be enhanced up to 443 mW cm-2.

    摘要 I Abstract II 致謝 III 目錄 VII 圖目錄 X 表目錄 XIV 符號表 XV 第一章 緒論 1 1.1 燃料電池源起及發展 1 1.2 燃料電池的種類 3 1.3 研究動機與目的 11 1.4 研究架構 12 第二章 文獻回顧 15 2.1 質子交換膜燃料電池之工作原理 15 2.1.1 電池的結構分析 16 2.1.2 雙極流場板 18 2.1.3 密封用膠片 19 2.1.4 氣體擴散層 19 2.1.5 微孔層 22 2.1.6 觸媒層 24 2.1.6.1 陽極觸媒材料 24 2.1.6.2 陰極觸媒材料 25 2.1.7質子交換膜 25 2.2 質子交換膜介紹 26 2.2.1 Nafion膜簡介及Nafion膜之改質系列 27 2.2.2 離子聚合物薄膜 31 2.2.3 酸/鹼高分子薄膜 32 2.2.4 有機/無機混成薄膜 32 2.2.5 高溫型質子交換膜 33 2.3 膜電極組內反應機制及製作方式 36 2.3.1 膜電極組內傳導機制 36 2.3.2電極放電的極化現象 38 2.3.3 觸媒製備 40 2.3.4 膜電極組製備方法 42 2.3.4.1 離子交換膜和觸媒之結合技術 42 2.3.4.2 氣體擴散層和觸媒之結合技術 44 2.3.5 觸媒漿料製作 48 2.4 電池操作因素對效能影響 49 2.4.1 操作溫度影響 49 2.4.2 陰極進料影響 50 2.4.3 進料濕度影響 50 2.4.4 氣體流量影響 50 2.4.5 進料背壓影響 50 2.4.6 熱壓程序影響 51 2.4.7 雙極流場板流道設計影響 51 2.5 聚乙烯醇的磺酸化、交聯反應 56 2.5.1 聚乙烯醇之簡介 56 2.5.2 磺酸化原理 56 2.5.3 聚乙烯醇磺酸化原理 57 2.6 4,4'-氧雙鄰苯二甲酸酐簡介 58 2.7 環氧樹脂簡介 58 2.8 薄膜的製備原理 60 第三章 實驗藥品、設備、原理及步驟 61 3.1 實驗藥品與設備 61 3.1.1 實驗材料與藥品 61 3.1.2 實驗設備與器材 64 3.2 實驗步驟 65 3.3 反應合成之流程與結構示意圖 69 3.4 實驗方法與儀器原理 72 3.4.1 薄膜結構鑑定 72 3.4.1.1 傅立葉轉換紅外光譜（FTIR）儀鑑定 72 3.4.1.2 固態核磁共振（NMR）光譜儀鑑定 73 3.4.2 熱性質之分析 74 3.4.3 物理性質之分析 75 3.4.3.1離子交換含量（IEC）測試 75 3.4.3.2含水率（Water uptake）及薄膜澎潤度（Swelling）測試 76 3.4.3.3示差掃瞄熱分析法（DSC） 77 3.4.3.4甲醇滲透率量測（Methanol permeability） 78 3.4.3.5元素分析（EA）儀分析 80 3.4.3.6機械性質測試（Mechanical properity） 80 3.4.4電化學性質之分析 81 3.4.4.1 AC-Impedance交流阻抗電化學特性測試 81 3.4.4.2燃料電池放電測試 84 3.4.4.2.1交換膜前處理 84 3.4.4.2.2 膜電極組之組裝步驟 85 3.4.4.2.3 電池放電測試 90 3.4.5薄膜型態分析 91 3.4.5.1穿透式電子顯微（TEM）鏡測量分析 91 3.4.5.2掃描式電子顯微鏡X光譜測量分析 91 第四章 實驗結果與討論 93 4.1 薄膜之結構鑑定 93 4.1.1 SOE薄膜之傅立葉轉換紅外光譜分析 93 4.1.2 NMR分析鑑定 97 4.2 薄膜之熱性質分析 100 4.2.1 SOE薄膜之熱裂解分析 100 4.3 薄膜之型態學分析 102 4.3.1 SOE薄膜之穿透式電子顯微鏡測量分析 102 4.3.2 SOE薄膜之表面型態與組成分析 105 4.4 薄膜之物理性質及導電度分析 108 4.4.1 SOE薄膜之含水率（Water uptake）、膨脹度（Sewlling）、離子交換當量（IEC）與元素分析（EA） 108 4.4.2 SOE薄膜之示差掃描分析 112 4.4.3 SOE薄膜之導電度 115 4.4.4 SOE薄膜甲醇滲透率量測 119 4.4.5 SOE薄膜機械性質測試 123 4.5 SOE薄膜之燃料電池探討及分析 125 4.5.1 氣體流量對電池性能之影響 125 4.5.2 操作溫度對電池性能之影響 127 4.5.3 壓合壓力對電池性能之影響 129 4.5.4 SOE薄膜測試結果討論 131 第五章 結論 139 第六章 未來研究方向 141 第七章 參考文獻 143

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