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研究生： 曹恩馨
Tsao, En-Hsin
論文名稱： 以中孔洞毛球型碳材為質子交換膜燃料電池陰極觸媒擔體之研究
Fluffy Mesoporous Carbon as Cathodic Catalyst Supports for Proton Exchange Membrane Fuel Cell
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： 2015
畢業學年度： 103
語文別： 中文
論文頁數： 143
中文關鍵詞： 質子交換膜燃料電池 、氧氣還原反應 、中孔洞碳材 、毛球型碳材
外文關鍵詞： Proton exchange membrane fuel cell (PEMFC), oxygen reduction reaction (ORR), mesoporous carbon, fluffy carbon
相關次數： 點閱：135  下載：1 
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    • 本研究在不同pH 環境下製備中孔洞碳粉，並以化學氣相沉積法成長奈米
    碳管，即為中孔洞毛球形碳材，探討在不同中孔洞碳粉種類下成長奈米碳管而得的觸媒擔體對質子交換膜燃料電池之陰極觸媒對於氧氣還原之活性的影響。
    其中中孔洞毛球型碳材的奈米碳管以強氧化劑部分拆鍊，使結構兼具奈米碳管及石墨烯的特性，以期獲得高導電度及高活性面積的特性，使氧氣還原活性提升。而毛球型碳材代表奈米碳管直接從碳粉主體生長，可增加碳材彼此之間的接觸點，亦可藉著奈米碳管連結其他片碳材，降低介面阻抗，增加電子傳遞效率。
    利用半電池系統分析探討氧化鐵吸附方式和時間、氧化鐵懸浮液濃度、碳
    管成長時間、乙炔濃度、奈米碳管拆鍊對觸媒活性的影響，並比較在不同pH中孔洞碳粉下的毛球型碳材，在不同氧化鐵溶液組成和乙炔濃度下對觸媒活性的影響。在氧化鐵吸附方式和時間條件中，以超音波震洗器和超音波細胞粉碎機兩種儀器做吸附能量差異的比較，吸附時間分為第一階段的分散氧化鐵奈米粒子集團，和第二階段的中孔洞吸附氧化鐵奈米粒子。震洗器和粉碎機的能量體積密度相差480 倍，當震盪時間過久或者瓦數過高時，都會使氧化鐵奈米粒子集團過度聚集而堵塞孔洞結構，造成表面積下降及質量活性下降。在氧化鐵懸浮液濃度的條件中，探討氧化鐵懸浮液體積和加入蒸餾水稀釋之後的總體積對觸媒活性的影響。當氧化鐵懸浮液體積越小，成長奈米碳管的數量越少；當總體積越大，奈米碳管的分散度越高。在碳管成長時間的條件中，發現成長時間越長，質量活性有下降的趨勢。
    以酸性製備中孔洞毛球型碳材而言，當粉碎機設定在100 瓦，氧化鐵溶液
    體積為1 ml，蒸餾水體積為10 ml，震盪的第一階段和第二階段皆為60 分鐘，碳管成長時間10 分鐘，乙炔濃度15%時，可以得到最高質量活性11.94 A/g Pt，是商用白金碳觸媒JM 的2.1 倍；以鹼性製備中孔洞毛球型碳材而言，根據上述相同條件，亦可以得到最高質量活性7.72 A/g Pt，是商用白金碳觸媒JM 的1.4 倍。整體而言，酸性製備中孔洞毛球型碳材可以得到較高的質量活性。

    Carbon nanotubes (CNT) were grown on mesoporous carbon (MC-CNT) by chemical vapor deposition with FeOx nanocatalyst. This type of fluffy mesoporous carbon 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 mesoporous carbon was also unzipped by modified Hummers' method and used rapid thermal reduction to remove oxygen functional group. The preparation parameters were during MC acidity preparation, FeOx adsorption methods into MC porous structure, FeOx
    adsorption time, CNT growth time, C2H2 concentration and effects of CNT unzipping.
    The highest mass activity at 0.65 V (vs. Ag/AgCl) was 11.94 A/g Pt in the research, which is 210% of that of commercial Pt/C catalyst, when FeOx was dispersed on an
    acid-synthesized mesoporous carbon for 60 minutes by ultrasonic processor, followed by CNT growth in 15% C2H2 at 650℃ for 10 minutes.

    摘要 I 致謝 X 目錄 XIV 圖目錄 XVIII 表目錄 XXII 第一章 緒論 1 1-1 前言 1 1-2 燃料電池簡介 1 1-2-1 歷史發展 2 1-2-2 燃料電池分類 3 1-2-3 燃料介紹 4 1-2-4 產業趨勢 6 1-3 質子交換膜燃料電池 8 1-3-1 電池結構 8 1-3-2 觸媒金屬粒子 10 1-3-3 觸媒擔體 11 1-3-3-1 中孔洞碳粉 12 1-3-3-2 奈米碳管 15 1-3-3-3 毛球碳材 16 1-3-3-4 拆鍊型奈米碳管 17 1-4 研究目的及論文內容 21 第二章 原理 22 2-1 質子交換膜燃料電池原理 22 2-1-1 氫氣氧化機制 23 2-1-2 氧氣還原機制 24 2-1-3 電池放電極化現象 25 2-2 觸媒製備原理 29 2-2-1 磁性氧化鐵奈米粒子 29 2-2-2 化學氣相沉積合成碳管 29 2-2-3 含浸還原法製備金屬粒子 31 2-3 電化學測試 32 2-3-1 循環伏安法 (Cyclic Voltammetry, CV) 32 2-3-2 線性掃描法 (Linear Sweep Voltammetry, LSV) 32 2-4 表面積及孔洞分析 33 2-4-1氮氣等溫吸脫附曲線 (N2 adsorption/desorption isotherm) 33 2-4-2 BET等溫吸附模式 36 2-4-3 BJH理論 37 第三章 實驗藥品及步驟 39 3-1 實驗藥品與儀器 39 3-2 中孔洞碳粉製備 41 3-3 氧化鐵懸浮液製備與表面修飾 42 3-4 以中孔洞碳粉成長奈米碳管 42 3-5 奈米碳管拆鍊 43 3-6 白金觸媒製備 44 3-7 觸媒之電化學活性分析 44 3-7-1 電池電極製備 44 3-7-2 半電池電化學測試活性 45 3-7-3 觸媒預活化 45 3-7-4 線性掃描法 46 3-8 單電池放電測試 46 3-8-1 質子交換膜 (Nafion 117) 前處理 46 3-8-2 參考電極製備 46 3-8-3 單電池漿料及觸媒層製備 48 3-8-4 膜電極組 (Membrane Electrode Assemble, MEA) 製備 49 3-8-5 單電池極化曲線分析 50 3-9 觸媒物理化學性質分析 51 3-9-1 表面積與孔洞分析 51 3-9-2 穿透式電子顯微鏡分析 51 3-9-3 掃描式電子顯微鏡分析 51 第四章 結果與討論 52 4-1 在酸中製備的碳粉上成長奈米碳管 52 4-1-1 氧化鐵奈米粒子吸附方式對觸媒活性的影響 56 4-1-2 氧化鐵奈米粒子吸附時間對觸媒活性的影響 66 4-1-2-1 以超音波振洗器吸附氧化鐵奈米粒子，不同時間組合對觸媒活性的影響 67 4-1-2-2 以超音波細胞粉碎機吸附氧化鐵奈米粒子，不同時間組合對觸媒活性的影響 77 4-1-3 氧化鐵奈米粒子懸浮液濃度對觸媒活性的影響 82 4-1-4 碳管成長時間對觸媒活性的影響 88 4-1-5 乙炔濃度對觸媒活性的影響 95 4-1-6 奈米碳管拆鍊對觸媒活性的影響 101 4-2 在鹼中製備的碳粉上成長奈米碳管 107 4-2-1 氧化鐵奈米粒子懸浮液濃度對觸媒活性的影響 111 4-2-2 乙炔濃度對觸媒活性的影響 121 4-3 綜合討論 127 4-3-1 不同碳粉下，氧化鐵奈米粒子懸浮液濃度的效應 128 4-3-2 不同碳粉下，乙炔濃度的效應 132 第五章 結論 136 第六章 參考文獻 138 第七章 附錄 143

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