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研究生： 施昱廷
Shih, Yu-Ting
論文名稱： 以拆鏈毛球碳材為質子交換膜燃料電池陰極觸媒載體之研究
Unzipped Fluffy Carbon as Cathodic Catalyst Supports for Proton Exchange Membrane Fuel Cells
指導教授： 楊明長
Yang, Ming-Chang
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： 2014
畢業學年度： 102
語文別： 中文
論文頁數： 166
中文關鍵詞： 質子交換膜燃料電池 、氧氣還原反應 、拆鏈 、毛球碳材
外文關鍵詞： Proton exchange membrane fuel cell (PEMFC), oxygen reduction reaction (ORR), unzipping, fluffy carbon
相關次數： 點閱：146  下載：1 
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    • 本研究以毛球碳材為基材進行拆鏈，以期獲得具有高導電性、高表面積的碳黑、奈米碳管及石墨烯的複合結構，做為質子交換膜燃料電池陰極觸媒擔體，以提高對於氧氣還原活性。
    本研究中將毛球碳材以改良的 Hummers' method進行氧化拆鏈，再以不同還原方式移除含氧官能基，此外也將拆鏈毛球碳材混摻聚乙烯吡咯烷酮（Polyvinylpyrrolidone, PVP），再經熱裂解後形成氮摻入拆鏈毛球碳材。
    本研究中拆鏈毛球碳材以碳管成長時間50分鐘、氧化劑與毛球碳材比例5 : 1及快速調溫還原在900oC持溫10分鐘為典型條件，探討碳管成長時間、拆鏈時氧化劑與毛球碳材比例對電化學活性的影響及最佳氧化石墨還原方式。研究結果顯示碳管成長50分鐘時，在0.65及0.7 V (vs. Ag/AgCl) 下具有最高質量活性為9.57及3.77 A/ gPt；在拆鏈時氧化劑與毛球碳材比例對電化學活性的影響方面，以氧化劑與毛球碳材比例5 : 1具有最高質量活性，在0.65及0.7 V (vs. Ag/AgCl) 下分別為9.57及3.77 A/ gPt；而在各種氧化石墨還原方法中，以快速調溫還原法製得之觸媒較其他還原方法製得之觸媒有較高的白金分散性及氧氣還原活性。針對快速調溫還原法的熱處理溫度及時間進行最佳化測試，結果顯示溫度1000oC持溫20分鐘下製得的拆鏈毛球碳材，具有最高比表面積714.7 m2/g和最高質量活性，在0.65及0.7 V (vs. Ag/AgCl) 下分別為9.95及4.01 A/ gPt，為本研究中氧氣還原活性最高的觸媒。
    此外，探討拆鏈毛球碳材混摻PVP時，混摻比例對氧氣還原活性的影響，在碳管成長時間50分鐘及氧化劑與毛球碳材比例5 : 1之拆鏈毛球碳材混摻PVP，並以快速調溫900及1000oC持溫10分鐘為典型條件下，混摻PVP與拆鏈毛球碳材比例8 : 1經1000oC裂解所得觸媒在0.65及0.7 V (vs. Ag/AgCl) 下具有較高質量活性為7.57及1.93 A/ gPt，但仍低於未混摻的結果，混摻效果並不佳。最後在單電池測試中，以半電池測試中質量活性最高的觸媒進行放電測試，所得最大放電功率為114.7 mW/cm2，為商用白金觸媒的117 %。

    Unzipped fluffy carbon (UFC) prepared by strong oxidation and rapid thermal reduction of fluffy carbon (FC) was explored as advanced cathodic catalyst supports to increase oxygen reduction reaction (ORR) activity for proton exchange membrane fuel cells (PEMFC). In this study, fluffy carbon was unzipped by modified Hummers' method and used rapid thermal reduction to remove oxygen functional group.
    The result indicated that UFC prepared by the condition of CNT growth time 50 min, oxidant to fluffy carbon ratio 5 : 1, and annealed at 1000oC for 20 min showed the highest surface area 714.7 m2/g and mass activity 9.95 and 4.01 A/g Pt at 0.65 and 0.7 V (vs. Ag/AgCl) in the research. In the single cell test results, the maximum power density of the best home-made catalysts (114.7 mW/cm2) is 117 % of that of commercial Pt/C catalsyt.

    摘要 I 誌謝 XI 目錄 XII 圖目錄 XVI 表目錄 XXVII 一、序論 1 1.1前言 1 1.2燃料電池簡介 1 1.2.1燃料電池起源與特色 1 1.2.2燃料電池種類 2 1.2.3 世界燃料電池發展概況 11 1.2.4 國外市場現況與趨勢 11 1.2.5 國內市場現況與趨勢 12 1.3質子交換膜燃料電池 16 1.3.1質子交換膜燃料電池基本構造 16 1.3.2質子交換膜 16 1.3.3觸媒金屬顆粒 17 1.3.4觸媒擔體 18 1.4研究目的 25 二、原理 26 2.1 氧氣還原反應 26 2.2 質子交換膜燃料電池工作原理 27 2.3 電池放電極化現象 28 2.3.1開環電壓 (EO)： 28 2.3.2 活性過電壓 29 2.3.3 歐姆過電壓 30 2.3.4 質傳過電壓 31 2.4 電化學分析方法 31 三、實驗方法 34 3.1 藥品 34 3.2 儀器設備 35 3.3 拆鏈毛球碳材 36 3.3.1毛球碳材之製備 36 3.3.2酸處理 38 3.3.3拆鏈毛球碳材製備 39 3.3.4還原方法 40 3.3.4.1 化學還原法 40 3.3.4.2 微波還原法 41 3.3.4.3 升溫還原法 42 3.3.4.4 快速調溫還原法 42 3.3.5氮摻入拆鏈毛球碳材製備 43 3.4電極漿料製備 44 3.4.1 Pt觸媒製備 44 3.4.2半電池電極製備 45 3.5 觸媒之電化學活性分析 45 3.5.1觸媒預活化 46 3.5.2線性掃描法 46 3.6 單電池放電測試 46 3.6.1 質子交換膜前處理 46 3.6.2 單電池參考電極製備 46 3.6.3 膜電極組熱壓製備 49 3.6.4 單電池極化曲線分析 50 3.7 觸媒物理化學性質分析 51 3.7.1 拉曼光譜分析 51 3.7.2 X光繞射儀分析 51 3.7.3 表面積與孔洞分析 51 3.7.4 穿透式電子顯微鏡分析 51 3.7.5 掃描式電子顯微鏡分析 52 3.7.6 化學分析電子光譜儀 52 四、結果與討論 53 4.1拆鏈後去除含氧官能基時還原方式比較 53 4.1.1穿透式電子顯微鏡分析 (TEM) 54 4.1.2能譜儀分析 (EDS) 56 4.1.3 X-射線繞射分析 (XRD)及顯微拉曼分析系統 (DXR) 57 4.1.4電化學活性測試 59 4.2毛球形碳材碳管成長時間比較及拆鏈的影響 63 4.2.1電子顯微鏡分析 (SEM) 63 4.2.2表面積與孔洞分析 (BET) 71 4.2.3顯微拉曼分析系統 (DXR) 71 4.2.4電化學活性測試 74 4.3氧化劑與毛球碳材比例 82 4.3.1電子顯微鏡分析 (SEM) 82 4.3.2能譜儀分析 (EDS)及表面積與孔洞分析 (BET) 85 4.3.3 X-射線繞射分析 (XRD)及顯微拉曼分析系統 (DXR) 86 4.3.4電化學活性測試 88 4.4熱處理溫度 92 4.4.1電子顯微鏡分析 (SEM) 92 4.4.2表面積與孔洞分析 (BET) 97 4.4.3顯微拉曼分析系統 (DXR) 98 4.4.4電化學活性測試 100 4.5熱處理時間 113 4.5.1顯微拉曼分析系統 (DXR) 113 4.5.2電化學活性測試 115 4.6經氮摻入的碳材 128 4.6.1電子顯微鏡分析 (TEM) 128 4.6.2化學電子能譜儀分析 (XPS) 及表面積與孔洞分析 (BET) 133 4.6.3顯微拉曼分析系統 (DXR) 137 4.6.4電化學活性測試 139 4.7綜合討論 147 4.7.1 單電池效能分析 147 4.7.2觸媒性質分析 152 五、結論 157 參考文獻 159 自述 166

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