為轉換及儲存地球上間歇性的可再生能源，電催化水裂解生產氫氣是人們致力研究具有前景的解決方法之一，在過去數十年內，低成本及高效率的雙功能水裂解催化劑被大量開發，其中又以Fe、Co、Ni金屬受到廣泛重視。因此，在本篇研究論文中，利用簡單的反微胞水熱合成法成功製備出FeCoNi2 NPs/Ni/NF催化劑，其具有巨孔結構的Ni奈米多面體陣列與奈米顆粒附著在表面，多層次的形貌使得催化劑可以有更多的活性中心暴露，提升電子傳遞和氣體排放通道。另外，金屬或非金屬元素的摻雜，除了改變材料形貌，在X射線光電子能譜和X射線吸收光譜的分析中，也證實電子組態有些許的差異，將這些材料調整添加時不同莫耳數比的金屬鹽或是氣體鍛燒時間，並利用電催化表現進行優化，以FeCoNi2Al0.2 NPs/Ni/NF電極的電催化效率最優異，不僅利用電阻值及電化學活性表面積解釋不同材料間催化活性的差異，其在1.0 M NaOH溶液中作為雙功能電極於整體水裂解，達到100和500 mA cm-2電流密度僅需要1.73 V及1.97 V電池電壓，且可以維持高電流密度表現長達60小時，法拉第電子轉換效率也趨近100%，顯示了該材料高度的電催化效率及穩定性。

In recent years, the intensive utilization of fossil fuels for human civilization has caused global warming and air pollution. Thus, developing a clean, renewable energy is a matter of utmost urgency. Electrochemical water splitting is recognized as one of the practical strategies for transforming sustainable energy sources, such as solar energy, into hydrogen fuel. It is essential to develop efficient and robust electrocatalysts for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER). Therefore, the development of earth-abundant, highly active electrocatalysts for overall water splitting is great importance. Currently, substantial effort has been made to design/synthesize Fe/Co/Ni-containing electrocatalysts responsible for promising catalytic activities and durability in HER and OER. In addition, by ways of heteroatom doping strategy, the optimization in morphology to expose more active sites and in electronic structure to improve the intrinsic activity was demonstrated for boosting water electrolysis efficiency. In this study, heteroatom-doped FeCoNi nanoparticles attached on Ni/NF substrate via a facile reverse-micelle hydrothermal strategy was successfully synthesized. The materials (denoted as FeCoNi2 NPs/Ni/NF) consist of interconnecting Fe/Co/Ni metallic nanocrystallites partially decorated by metal (Al) or non-metal (N, P). After assessing 14 kinds of FeCoNi-based catalysts for overall water splitting, FeCoNi2Al0.2 NPs/Ni/NF catalyst exhibits superior bifunctional electrocatalytic performances. Water electrolyzer employing FeCoNi2Al0.2 NPs/Ni/NF as both the anode and cathode delivers high current densities of 100 and 500 mA cm-2 at low cell voltages of 1.73 V and 1.97 V in 1.0 M NaOH aqueous solution, respectively. Presumably, the excellent bifunctional electrocatalytic properties of FeCoNi2Al0.2 NPs/Ni/NF could be ascribed to high conductivity, minimum charge transfer resistance, and maximum active surface area.

摘要 i
Abstract ii
謝誌 iii
目錄 iv
圖目錄 vii
表目錄 xiii
第一章 緒論 1
1-1. 能源 1
1-2. 電催化水裂解 3
1-2-1. HER基本反應機制 4
1-2-2. OER基本反應機制 6
1-2-3. 電催化劑效率評估參數 7
1-3. 貴重金屬 10
1-3-1. Pt金屬應用於HER 11
1-3-2. Ir金屬應用於OER 13
1-4. 地球富含的過渡金屬 15
1-5. 常見的電催化劑表面結構 16
1-5-1. 電沉積薄膜 (Electrodeposition-film) 16
1-5-2. 奈米層片 (Nanosheets) 18
1-5-3. 奈米柱 (Nanorods) 20
1-5-4. 奈米管 (Nanotubes) 22
1-5-5. 奈米立方 (Nanocubes) 23
1-5-6. 奈米顆粒 (Nanoparticles) 24
1-6. 過渡金屬摻雜異原子 26
1-6-1. 摻雜鋁的電催化劑 26
1-6-2. 摻雜氮的電催化劑 29
1-6-3. 摻雜磷的電催化劑 32
1-7. 奈米顆粒的製備 35
1-8. 研究方向 37
第二章 實驗部分 38
2-1. 一般實驗 38
2-2. 合成設備介紹水 38
2-2-1. 熱合成反應器 (Hydrothermal Autoclave Reactor) 38
2-2-2. 管型高溫爐 (Tube Furnaces) 39
2-3. 儀器與方法 40
2-3-1. 高解析光電子能譜儀 (High Resolution X-ray Photoelectron Spectrometer, XPS) 40
2-3-2. 熱場發射掃描式電子顯微鏡 (Thermal type Field Emission Scanning Electron Microscope, FESEM) 41
2-3-3. 高解析穿透式電子顯微鏡 (High Resolution Transmission Electron Microscope, HRTEM) 41
2-3-4. 雙束聚焦離子束顯微鏡 (Dual-Beam Focused Ion Beam, DB-FIB) 42
2-3-5. 能量色散X射線光譜 (Energy-Dispersive X-ray Spectroscopy, EDX) 42
2-3-6. 感應耦合電漿質譜分析儀 (Inductively Coupled Plasma-Mass Spectrometry, ICP-MS) 43
2-3-7. 粉末X光繞射儀 (Powder X-ray Diffraction, PXRD) 43
2-3-8. 拉曼光譜儀 (Raman Spectrometer) 44
2-3-9. X射線吸收光譜儀 (X-ray Absorption Spectroscopy, XAS) 44
2-3-10. 軟X射線吸收光譜儀 (Soft X-ray Absorption Spectroscopy, Soft XAS) 45
2-3-11. 循環伏安儀 (Cyclic Voltammetry, CV) 45
2-3-12. 電化學阻抗分析儀 (Electrochemical Impedance Spectroscopy, EIS) 46
2-3-13. 氣象層析儀 (Gas Chromatography, GC) 46
2-4. 溶劑與藥品 47
2-4-1. 溶劑 47
2-4-2. 藥品 47
2-4-3. 高溫爐氣體 48
2-5. 催化劑合成 49
2-5-1. 合成FeCoNi2 NPs 49
2-5-2. 合成Ni(OH)2 NS/NF 51
2-5-3. 合成Ni/NF 52
2-5-4. 合成FeCoNi2 NPs/Ni/NF 52
2-5-5. 合成FeCoNi2Al0.2 NPs/Ni/NF 53
2-5-6. 合成FeCoNi2Nx NPs/Ni/NF 53
2-5-7. 合成FeCoNi2Px NPs/Ni/NF 54

2-6. 製備催化劑電極板 55
2-6-1. 泡沫鎳暴露面積 55
2-6-2. 奈米顆粒滴落塗布於電極板 55
2-7. 電化學 56
2-7-1. 電化學催化效率表現 56
2-7-2. 電化學電容(Capacitance) 57
2-7-3. 電化學阻抗分析(EIS) 58
2-7-4. 法拉第效率(Faradaic efficiency) 59
第三章 結果與討論 61
3-1. FeCoNi Bulk與Nanoparticle的比較 61
3-1-1. 電催化活性 61
3-1-2. 本質催化活性 63
3-1-3. 催化劑電極設計 65
3-2. 基材Ni/NF之鑑定 66
3-3. FeCoNi2 NPs/Ni/NF之鑑定與電催化表現 68
3-3-1. 材料鑑定 68
3-3-2. 電催化表現 76
3-4. FeCoNi2Al0.2 NPs/Ni/NF之鑑定與電催化表現 84
3-4-1. 材料鑑定 84
3-4-2. 電催化表現 93
3-5. X射線吸收光譜分析 97
3-5-1. X射線吸收近緣結構 97
3-5-2. 延伸X射線吸收精細結構 99
3-6. FeCoNi2Nx NPs/Ni/NF及FeCoNi2Px NPs/Ni/NF之鑑定與電催化表現 106
3-6-1. 材料鑑定 106
3-6-2. 電催化表現 117
3-7. 電化學評估 123
3-7-1. 電催化表現總比較 123
3-7-2. 電化學活性表面積 129
3-7-3. 電荷轉移電阻 132
3-7-4. 整體水裂解穩定性 135
3-7-5. 法拉第效率 136
第四章 結論 137
參考文獻 139

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