為了滿足不斷增長的能源需求、降低汙染水平、發展乾淨且可持續再生的能源是現代社會不可避免的議題。燃料電池由於其高轉換效率而成為最有前景的能量轉換裝置之一。陰極的氧氣還原反應 (Oxygen Reduction Reaction) 在燃料電池所有組件中佔有最高的能障 (energy barrier) ，因此需要奈米觸媒 (NCs) 來增強緩慢的反應動力學。鉑基奈米觸媒的高製造成本和電化學活性是開發需要高可靠度及符合成本效益的燃料電池會面臨到的主要瓶頸。因此，為了有效降低奈米觸媒成本並同時提高ORR性能，我們開發了一系列的奈米碳管承載四元多尺度混合金屬奈米觸媒，使其具有鈷錫鈀三元層次結構與原子級鉑團簇修飾結構缺陷。另外，使用簡單快速的濕式化學還原法，並利用不同比例的鉑 (0.5 - 3 wt%) 進行修飾。透過交叉參考X光光譜 (XRD及XAS) 和電化學分析的結果，我們證明了添加錫 (Sn) 會增加原子半徑與表面能，因此鉑 (Pt) 原子會傾向於填充多金屬界面或表面缺陷等表面能較高的位置，同時表面修飾的鉑團簇會從鄰近電負度較低的原子得到電子。這些效應能有效地提升四元多層次結構奈米觸媒 (NCs) 的質量活性 (MA) 和0.85 V的動力學電流值 (Jk) ，且與商業用鉑觸媒 (J.M.Pt/C) 性能相比，當鉑 (Pt) 為1 wt%時，MA提高了20倍 (2146.2 mAmgPt -1) 。
本研究製備出的原子級鉑團簇修飾鈷錫鈀層次結構之四元混合金屬奈米觸媒，藉由調整鉑修飾比例、錫鈀比例與厚度、鈷與酸化奈米碳管之擴散溫度，瞭解鉑原子團簇在不同結構上的變化與對氧氣還原反應活性之間的關聯。如此一來，便能有效地增加催化電流與觸媒反應活性，並減少鉑金屬使用量以降低成本，這種具有預期性能的材料設計方式可以加速發展具有高活性的鉑金屬修飾過渡金屬基觸媒的開發。

In order to meet the growing energy demand, reduce pollution levels, and develop clean and sustainable renewable energy is an inevitable issue in modern society. Fuel cells are one of the most promising energy conversion devices due to their high conversion efficiency. The Oxygen Reduction Reaction of the cathode occupies the highest energy barrier in all components of the fuel cell, so nanocatalysts (NCs) are required to enhance the slow reaction kinetics. The high manufacturing cost and electrochemical activity of platinum-based nanocatalysts are the main bottlenecks faced by fuel cells that require reliability and cost. Therefore, in order to effectively reduce the cost of nanocatalysts and improve the performance of ORR, a series of acidic carbon nanotubes are loaded with a quaternary hierarchical mixed metal nanocatalyst, which has a cobalt-tin-palladium ternary hierarchical structure with atomic platinum cluster modified structural defects. By using a simple but rapid wet chemical reduction method, Co/SnO2/Pd hierarchical structure nanocatalysts with different amount of platinum (0.5 - 3 wt%) can be synthesized. Through cross-reference X-ray spectroscopy (XRD and XAS) and electrochemical analysis, we show that the addition of tin (Sn) increases the atomic radius and surface energy, so platinum (Pt) atoms tend to grow on polymetallic interfaces or surface defects, which has a higher surface energy. Surface-decorated platinum clusters will receive electrons from adjacent atoms with lower electronegativity. These effects can effectively improve the mass activity (M.A.) of quaternary multi-layer nanocomposites (NCs) and the kinetic current value (Jk) of 0.85 V, compared to commercial platinum catalyst (J.M.Pt/C) performance. When the platinum loading is 1 wt%, the MA is increased by 20 times (1345.9 mAmgPt -1) .
The atomic platinum clusters prepared in this experiment modify the cobalt-tin-palladium hierarchical quaternary mixed metal nanocatalyst by adjusting the platinum modification ratio, the ratio of tin to palladium and the thickness, and the diffusion temperature of cobalt and acidic carbon nanotubes. The relationship between platinum atomic clusters in different structures and the activity of oxygen reduction reaction can effectively increase the kinetic current and catalyst activity, and reduce the usage of platinum metal to reduce the cost. Identifying materials design with expected properties can accelerate the development of highly active and abundant transition-metal-based catalysts with low platinum loading

目錄
內容
摘要 i
英文摘要 ii
誌謝 iv
目錄 v
表目錄 vi
圖目錄 viii
第一章 緒論 14
1-1 研究背景 14
1-2 燃料電池產業及發展 16
1-3 燃料電池種類 18
1-3-1 固態氧化物燃料電池 (Solid Oxide Fuel Cell, SOFC) 18
1-3-2 熔融碳酸鹽燃料電池 (Molten Carbonate Fuel Cell, MCFC) 19
1-3-3 磷酸燃料電池 (Phosphoric Acid Fuel Cell, PAFC) 19
1-3-4 質子交換膜燃料電池 (Proton Exchange Membrane Fuel Cell, PEMFC) 19
1-3-5 鹼性燃料電池 (Alkaline Fuel Cell, AFC) 20
1-4 鹼性燃料電池發展瓶頸 21
1-5 鹼性燃料電池之工作原理 23
1-6 氫氣氧化反應 (Hydrogen oxidation reaction；HOR) 29
1-7 氣氣還原反應 (Oxygen Reduction Reaction, ORR) 30
1-8 影響觸媒活性的因素 35
第二章 文獻回顧 36
2-1 觸媒發展方向 36
2-2 觸媒的大小與形貌對於氧氣還原活性的影響 37
2-3 影響鉑原子級團簇使用率的因素 41
2-4 影響鉑團簇結構的因素 44
2-5 文獻回顧總結 50
第三章 實驗方法 52
3-1 前言 52
3-2 實驗設計 53
3-2-1 實驗研究方向 53
3-2-2 實驗藥品 55
3-2-3 奈米碳管酸處理 55
3-3 實驗流程 56
3-4 材料特性 61
3-5 電化學分析 62
3-5-1 循環伏安法 (Cyclic voltammetry, CV) 64
3-5-2 線性掃描伏安法 (Linear Sweep Voltammetry, LSV) 66
3-5-3 電化學阻抗圖 (Electrochemical impedance spectroscopy, EIS) 69
3-6 物性分析 73
3-6-1 穿透式電子顯微鏡 (Transmission electron microscope, TEM) 73
3-6-2 X光繞射分析儀 (X-ray diffraction, XRD) 75
3-6-3 X射線吸收光譜 (X-ray absorption spectroscopy, XAS) 78
3-6-4 X光光電子能譜 (X-Ray Photoemission Spectroscopy, XPS) 83
3-6-5 感應耦合電漿分析 (Inductively Coupled Plasma, ICP) 84
第四章 結果與討論 86
4-1 不同鉑金屬含量修飾奈米觸媒對氧氣還原活性之影響 86
4-1-1 電化學分析 88
4-1-2 表面形態和晶體結構 95
4-1-3 本節總結 112
4-2 不同鈀錫比例之殼層對氧氣還原活性之影響 113
4-2-1 電化學分析 115
4-2-2 表面形態和晶體結構 119
4-2-3 本節總結 129
4-3 不同鈷與奈米碳管之攪拌溫度對氧氣還原活性之影響 130
4-3-1 電化學分析 132
4-3-2 表面形態和晶體結構 136
4-3-3 本節總結 148
第五章 結論 149
參考文獻 150

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