奈米複合電極觸媒材料的製備與鑑定｜國立清華大學博碩士論文庫

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研究生：	曾友利 Tze, You-Li
論文名稱：	奈米複合電極觸媒材料的製備與鑑定 Preparation and characterization of nanocomposite electrode catalysts
指導教授：	楊家銘 Yang, Chia-Min
口試委員:
學位類別：	碩士 Master
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2009
畢業學年度：	97
語文別：	中文
論文頁數：	107
中文關鍵詞：	甲醇燃料電池、陽極觸媒、鉑、金屬氧化物、高分子
外文關鍵詞：	DMFC, Anodic catalyst, Pt, Metal oxide, Polymer
相關次數：	點閱：3 下載：0
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本論文目的在製備奈米複合電極觸媒並鑑定其活性，我們以SBA-15為模板合成中孔洞碳材：CMK-3，接著以CMK-3為支架形成複合高分子/CMK-3材料，利用不同的複合高分子/CMK-3為載體，以膠體法及乙二醇還原法合成甲醇燃料電池陽極觸媒。另外為了增進催化活性，也添加TiO2或是CeO2於複合高分子碳材再以乙二醇還原製備陽極觸媒。上述的材料以X光粉末繞射儀、氮氣物理吸脫附儀、熱分析儀做結構鑑定。陽極觸媒的活性則以循環伏安法分析甲醇氧化及一氧化碳剝除實驗來判斷。結果顯示以複合親水性的高分子CMK-3為載體可提高觸媒活性，但在0.8V運作大約30分鐘電流強度下降約40% ~ 50%。而添加TiO2或是CeO2後催化電流強度與觸媒的穩定性相較於未添加前都有明顯的提升。

In this thesis we have aimed at the preparation and characterization of nanocomposite electrocatalysts for direct methanol fuel cell (DMFC). We applied mesoporous SBA-15 silica as a hard template to prepare mesoporous CMK-3 carbon, which were then used to prepared polymer/CMK-3 nanocomposites. Pt nanoparticles were then reduced and deposited on the nanocomposites by the colloidal method or alcohol reduction method. Alternatively, metal oxides including TiO2 and CeO2 were added into the nanocomposites, with the attempt to enhance the electroactivity of Pt nanoparticles. The thus prepared nanocomposite materials were characterized by X-ray diffraction, nitrogen physisorption analysis, and thermal analysis. Besides, the electrochemical activities of the Pt-containing nanocomposite catalysts were analyzed by cyclic voltammetry and CO-stripping experiments. The results showed that the catalytic activity got better when using polymer/CMK-3 nanocomposites containing hydrophilic polymers. However, these nanocomposite catalysts also exhibited 40-50% decrease in current density of methanol oxidation at 0.8 V after running the half cells for around 30 min. On the other hand, the addition of TiO2 or CeO2 indeed enhance the performance of the Pt-containing nanocomposites, which exhibited higher current density and better stability.

中文摘要............................. Ⅰ
英文摘要............................. Ⅱ
目錄................................. Ⅲ
圖目錄............................... Ⅶ
表目錄............................... ⅩⅠ

第一章 緒論.................................... 1
1-1 燃料電池簡介............................... 2
1-2 直接甲醇燃料電池........................... 5
1-2-1 DMFC 的工作原理.......................... 6
1-2-2 DMFC 的極化現象.......................... 7
1-2-3 DMFC 的構造.............................. 10
1-3 陽極觸媒................................... 12
1-3-1 陽極觸媒的催化機制....................... 12
1-3-2 雙金屬或多金屬的陽極觸媒................. 14
1-3-3 添加金屬氧化物的陽極觸媒................. 21
1-3-4 陽極觸媒的載體........................... 23
1-3-5 陽極觸媒的製備方法....................... 28
1-4 研究動機及目的............................. 32

第二章 實驗部分................................ 34
2-1 實驗藥品................................... 34
2-2 SBA-15 的合成.............................. 36
2-3 中孔洞碳材之合成........................... 37
2-4 複合高分子/CMK-3 中孔洞碳材的合成.......... 38
2-5 以不同高分子/ CMK-3 複合材料為載體合成觸媒. 39
2-5-1 不同高分子/CMK-3 複合材料的合成.......... 39
2-5-2 添加CeO2 至高分子/CMK-3 複合材料的合成... 40
2-5-3 添加TiO2 至高分子/CMK-3 複合材料的合成... 40
2-5-4 以膠體法合成陽極觸媒材料................. 40
2-5-5 以乙二醇還原法合成陽極觸媒材料........... 41
2-6 儀器鑑定與分析............................. 43
2-6-1 X 光粉末繞射光譜儀....................... 43
2-6-2 氮氣物理吸附儀........................... 45
2-6-3 熱重分析儀............................... 51
2-6-4 穿透式電子顯微鏡......................... 52
2-6-5 循環伏安法............................... 53

第三章 結果與討論.............................. 57
3-1 SBA-15 與CMK-3 的合成與鑑定................ 57
3-1-1 SBA-15 的合成與鑑定...................... 59
3-1-2 CMK-3 的合成與鑑定....................... 62
3-2 高分子/CMK-3 複合材料的合成與鑑定.......... 66
3-2-1 PXRD 分析................................ 67
3-2-2 氮氣物理吸脫附分析....................... 68
3-2-3 熱重分析................................. 69
3-3 CMK3-nX-Pt(Z)陽極觸媒的合成與鑑定.......... 71
3-3-1 膠體法合成陽極觸媒....................... 72
3-3-1-1 PXRD 分析.............................. 72
3-3-1-2 循環伏安法分析......................... 74
3-3-1-3 計時安培伏安法分析..................... 78
3-3-1-4 一氧化碳剝除實驗....................... 79
3-3-2 乙二醇還原法合成陽極觸媒................. 80
3-3-2-1 PXRD 分析.............................. 81
3-3-2-2 循環伏安法分析......................... 83
3-3-2-3 計時安培伏安法分析..................... 85
3-3-2-4 一氧化碳剝除實驗....................... 86
3-4 CMK3-0.33Si-Y-Pt(EG) 陽極觸媒的合成與鑑定.. 88
3-4-1 PXRD 與熱重分析.......................... 89
3-4-2 TEM 鑑定................................. 91
3-4-3 循環伏安法分析........................... 93
3-4-4 計時安培伏安法分析....................... 94
3-4-5 一氧化碳剝除實驗......................... 96
第四章 結論.................................... 97
第五章 參考文獻................................ 99

圖目錄
圖1-1 氧化還原轉換電能現象..................... 2
圖1-2 DMFC 工作示意圖.......................... 7
圖1-3 DMFC 的極化曲線圖........................ 8
圖1-4 Nafion-117® 結構圖...................... 10
圖1-5 DMFC 陽極觸媒催化機制示意圖............. 13
圖1-6 不同比例得合金觸媒對於CO 的氧化電位..... 15
圖1-7 Pt, Ru 與PtRu 觸媒在0.1 M過氯酸下進行CO
的剝除實驗.................................... 16
圖1-8 Pt, Ru 與Pt-Ru 觸媒在1 M 甲醇與0.1 M 過
氯酸溶液中的線性伏安掃描...................... 16
圖1-9 PtRu 合金觸媒催化甲醇反應示意圖......... 17
圖1-10 PtRu 非合金的兩種極端分布情形.......... 18
圖1-11 合金觸媒穩態電流對應電壓值之比較....... 20
圖1-12 CMK-3 合成示意圖....................... 26
圖1-13 CMK-3 的孔洞結構....................... 26
圖1-14 複合高分子CMK-3 材料形成示意圖......... 27
圖1-15 PS-CMK-3 與CMK-3 之導電度比較.......... 28
圖1-16 PS-TiPOSS/SBA-15 材料合成示意圖........ 32
圖2-1 高分子聚合步驟示意圖.................... 39
圖2-2 布拉格繞射示意圖........................ 43
圖2-3 SBA-15 的XRD 圖......................... 44
圖2-4 Type Ⅳ吸附曲線型態示意圖............... 46
圖2-5 四種遲滯曲線的型態示意圖................ 46
圖2-6 圓柱型孔洞示意圖........................ 49
圖2-7 QuantachromeAutosorb – 1MP 系統裝置圖.. 51
圖2-8 熱重分析裝置圖.......................... 52
圖2-9 循環伏安示意圖.......................... 54
圖2-10 電化學量測裝置圖....................... 54
圖3-1 糠醇分子結構圖.......................... 57
圖3-2 模板中孔洞碳材合成過程.................. 57
圖3-3 SBA-15 之PXRD 圖........................ 60
圖3-4 SBA-15 熱重分析圖....................... 60
圖3-5 SBA-15-cal 氮氣物理吸脫附及BJH 孔徑分布圖. 61
圖3-6 糠醇聚合反應機制........................ 62
圖3-7 CMK-3 與SBA-15-cal 之PXRD 圖............ 63
圖3-8 CMK-3 氮氣物理吸脫附及BJH 孔徑分布圖.... 64
圖3-9 CMK-3 熱重分析圖........................ 65
圖3-10 高分子中孔洞碳複合材料合成示意圖....... 68
圖3-11 CMK-3-p 系列之PXRD 圖.................. 67
圖3-12 CMK-3-p 系列之氮氣物理吸脫附及BJH 孔徑
分布圖........................................ 68
圖3-13 CMK-3-p 系列熱重分析圖................. 70
圖3-14 CMK3-nX-Pt(Col) 系列之小角與廣角PXRD 圖 73
圖3-15 CMK3-nX-Pt(Col) 系列之循環伏安法分析圖. 75
圖3-16 (a) TEVS 與(b) 4-VPy 於陽極觸媒中之示意圖 77
圖3-17 CMK3-nX-Pt(Col) 系列之計時安培伏安法分析圖 79
圖3-18 CMK3-nX-Pt(Col) 系列之一氧化碳剝除實驗圖 80
圖3-19 EG 作還原劑機制........................ 81
圖3-20 CMK3-nX-Pt(EG) 系列之小角與廣角PXRD 圖  82
圖3-21 CMK3-nX-Pt(EG) 系列之循環伏安法分析圖.. 84
圖3-22 CMK3-nX-Pt(EG) 系列之計時安培伏安法分析圖 85
圖3-23 CMK3-nX-Pt(EG) 系列之一氧化碳剝除實驗圖 87
圖3-24 CMK3-0.33Si-Y-Pt(EG) 系列之小角與廣角
PXRD圖........................................ 89
圖3-25 CeO2 在EG 中的溶解反應................. 90
圖3-26 CMK3-0.33Si-Y-Pt(EG) 系列之熱重分析圖.. 91
圖3-27 CMK3-0.33Si-TiO2-Pt(EG) 之TEM 圖....... 92
圖3-28 CMK3-0.33Si-CeO2-Pt(EG) 之TEM 圖....... 93
圖3-29 CMK3-0.33Si-Y-Pt(EG) 系列之循環伏安法分
析圖.......................................... 93
圖3-30 CMK3-0.33Si-Y-Pt(EG) 系列之計時安培伏安
法分析圖.......................................95
圖3-31 CMK3-0.33Si-Y-Pt(EG) 系列之一氧化碳剝除
實驗圖.........................................96

表目錄
表1-1 各種燃料電池之比較....................... 4
表1-2 氫氣與甲醇在不同儲存方式下的能量密度..... 5
表1-3 不同的觸媒載體性質...................... 24
表2-1 樣品總表................................ 42
表3-1 樣品簡稱................................ 58
表3-2 SBA-15 和CMK-3 氮氣物理吸脫附數據....... 64
表3-3 複合材料樣品簡稱........................ 66
表3-4 高分子中孔洞碳複合材料之氮氣吸脫附數據.. 69
表3-5 CMK3-nX-Pt(Z) 樣品簡稱.................. 71
表3-6 CMK3-nX-Pt(Col) 系列之電化學數據........ 76
表3-7 CMK3-nX-Pt(EG) 系列之PXRD 數據.......... 83
表3-8 CMK3-nX-Pt(EG) 系列之電化學數據......... 84
表3-9 CMK3-nX-Pt(Z) 樣品簡稱.................. 88
表3-10 CMK3-0.33Si-Y-Pt(EG) 系列之電化學數據.. 94

                                

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