隨著能源耗竭與環境保護議題逐漸受到人們的重視，發展乾淨的替代性能源為當前亟需加速研究之目標。電解水產氫被視為下一個世代潔淨且高純度之綠色能量來源，也因此，開發長壽高效穩定之電化學觸媒在整個領域中扮演相當重要的角色。目前為止，白金被視為最優異之產氫觸媒材料，而二氧化銥與二氧化釕為表現最佳之產氧觸媒材料。然而，這些金屬因地殼蘊藏量稀少且價格昂貴，在商業能源發展上受到極大的限制。所以，目前研究無不希望找尋價廉穩定高效之電觸媒為實現綠色能源之應用。
在已知材料當中，鐵鈷鎳銅鉬等過渡金屬與其衍生物被視為最有潛力之催化元素，因其電子價態性質與價格低廉之優勢，在許多電化學觸媒領域被廣泛的使用。在奈米材料製備方面，金屬奈米線陣列和反蛋白石奈米結構因其規則有序且具高比表面積之特性、孔洞易於氣體氣泡之排除、且利於加速電子傳遞速率，適合用於電解水電極之開發。因此，綜合以上討論，本篇研究分別以商用多孔陽極氧化鋁薄膜和聚苯乙烯奈米球為模板，成功合成鎳鐵核/硫化鎳鐵殼奈米線陣列和鎳鐵鉬合金反蛋白石結構於泡沫鎳上，並將兩奈米材料用於電解水產氫之催化應用上。
在電化學表現方面，以1M氫氧化鉀作為電解質，鎳鐵核/硫化鎳鐵殼奈米線陣列在陽極產氧端表現優異，並提供電觸媒材料設計一個新的發展基礎。另一方面，鎳鐵鉬合金反蛋白石結構成長於泡沫鎳上，用作產氫產氧雙效觸媒表現突出，為已知雙效電解水觸媒當中，高電流條件下表現最佳之材料。並在長時間嚴苛條件操作下，仍能保持其催化活性。所有測試無不顯示本研究開發之兩觸媒材料具備優異之電催化性質，並期待在未來商業能源電解水產氫發展中展現其潛力，以體現最終潔淨能源之目標。

Because of elevating energy demand and worsening environmental pollution, development of clean alternative energies has become the top priority of scientific research efforts. Hydrogen production from renewable energy driven electrolytic water splitting is considered a promising technology for supply of clean alternative energy. Among other things, development of stable and efficient catalysts for electrolytic water splitting has drawn extensive and intensive research attention. Platinum is reported to be the most efficient catalyst for hydrogen evolution reactions (HER), whereas iridium oxide is regarded as a benchmarking catalyst for oxygen evolution reactions (OER). Nevertheless, because of the scarcity and extremely high cost of Pt and Ir, it is not promising for them to realize large scale commercial applications. Therefore, developing efficient, stable, and non-precious metal-based catalysts is urgently needed.
Transition metals, including iron, cobalt, nickel, copper, and molybdenum, and their derivatives are viewed as promising catalyst materials and have been intensively investigated for electrolytic water splitting. On the other hand, metal nanowire arrays and metal inverse-opal structure have caught a lot of research attention because of their ordered structure and high surface areas for targeted reactions. These advantageous characteristics significantly enhance the relevant electrochemical performances because of the enhanced charge transport path and bubble escape. With all the factors mentioned above, core/shell NiFe/sulfurized NiFe (NiFe/S-NiFe) nanowire arrays and NiFeMo inverse-opal structure on nickel foam have been successfully fabricated with anodic aluminum oxide membranes (AAO) and self-assembled polystyrene (PS) spheres on nickel foam backbone surfaces as the templates, respectively.
In terms of the electrocatalytic performances, NiFe/S-NiFe nanowire arrays show outstanding potentials for oxygen evolution reactions. On the other hand, NiFeMo inverse-opal structure on nickel foam shows excellent bifuctional electrcatalytic performance. It outperforms most of the bifuctional catalysts for overall water splitting at high current densities. Notably, the two catalysts developed here exhibit excellent durability. The present development proves to be a promising new catalyst architecture design for electrocatalytic processes.

摘要 I
致謝 IV
總目錄 V
圖目錄 VIII
表目錄 XII
第一章緒論 1
1.1 前言 1
1.2 電催化分解水反應機制 1
1.3 反應之過電位 4
1.4電化學三極式量測裝置 5
1.4.1參考電極 5
1.4.2對電極 6
1.5常見的OER與HER觸媒 7
1.5.1鎳鐵金屬材料 7
1.5.2金屬硫化物 8
1.5.3鉬金屬與其衍生物 9
1.6 以AAO為模板生成之金屬奈米線 9
1.7 商用泡沫鎳於電解水領域之應用 10
1.8 以聚苯乙烯奈米球為模板生成之反蛋白石結構 10
1.9 研究動機 11
第二章文獻回顧 13
2.1 鎳鐵金屬與其硫化物於OER之應用 13
2.1.1 鎳鐵金屬於OER之應用 13
2.1.2金屬硫化物於OER之應用 17
2.2鎳鐵金屬與其硫化物於HER之應用 19
2.3 鉬金屬與其衍生物用於HER及OER之應用 21
2.4 以AAO為模板基礎電鍍合成鎳鐵金屬奈米線 25
2.5 以聚苯乙烯奈米球為模板合成反蛋白石結構用於電解水觸媒 27
第三章實驗方法 29
3.1 實驗藥品 29
3.2 實驗器材 31
3.3 材料分析儀器 31
3.4 實驗方法與步驟 33
3.4.1 鎳鐵合金奈米線陣列製作 33
3.4.2 硫化鎳鐵合金奈米線陣列 34
3.4.3 鎳鐵鉬合金反蛋白石結構成長於泡沫鎳骨幹 35
3.5 電化學性質量測 36
3.5.1 HER和OER過電位之量測 37
3.5.2 電化學阻抗頻譜分析法(EIS) 37
3.5.3 全電極系統電化學量測(Full Cell Measurement) 38
3.5.4 長效性測試(Long-term Stability Test) 38
第四章結果與討論 40
4.1 鎳鐵核/硫化鎳鐵殼奈米線陣列之材料分析 40
4.1.1 鎳鐵合金奈米線陣列 40
4.1.2 鎳鐵核/硫化鎳鐵殼奈米線陣列 45
4.2 鎳鐵核/硫化鎳鐵殼奈米線陣列之電化學性質分析 53
4.2.1 奈米線陣列OER之電化學表現 53
4.2.2 奈米線陣列HER之電化學表現 57
4.2.3 奈米線陣列組成全電解水系統之電化學表現 60
4.3 鎳鐵核/硫化鎳鐵殼奈米線陣列與其他文獻活性表現整理 65
4.4 鎳鐵鉬合金反蛋白石結構成長於泡沫鎳之材料分析 68
4.5 鎳鐵鉬合金反蛋白石結構成長於泡沫鎳之電化學性質分析 74
4.5.1 鎳鐵鉬合金反蛋白石結構OER之電化學表現 75
4.5.2 鎳鐵鉬合金反蛋白石結構HER之電化學表現 81
4.5.3 鎳鐵鉬合金反蛋白石結構組成全電解水系統之電化學表現 86
4.6 鎳鐵鉬合金反蛋白石結構成長於泡沫鎳與其它文獻活性表現整理 94
第五章結論 96
參考文獻 97

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