以電化學沉積法合成鎳基含磷化合物複合電觸媒材料，並且測試其在1 M KOH的鹼性條件下應用於產氫反應的電化學測試。鎳基含磷化合物複合電觸媒材料的微結構分析、成分元素分析等等物性分析，將利用掃描式電子顯微鏡(SEM)、能量散射光譜儀(EDS)、感應耦合電漿原子發射光譜儀(ICP-OES)和X光吸收光譜(XAS)等儀器作定性與定量分析；電化學性質分析將利用循環伏安法(CV)、線性掃描伏安法(LSV)和計時伏安法(Chronovoltammetry)等電化學分析方法。藉由探討電鍍電流密度與電鍍液之鎳磷組成比例找出最佳電催化活性的電鍍條件。在探討電鍍電流密度中了解隨著電流密度越強，鎳基電觸媒的球狀結構會越小，可以控制球徑大小750 nm至250 nm，另一方面，造成電化學活性表面積越大，觸媒活性與交換電流密度也越好，其中以-20000 μA cm-2電流密度為最佳條件，過電位與交換電流密度分別是176±1.3 mV與-5.3±0.1 μA cm-2。在電鍍液組成比例探討中，各組成比例合成之電觸媒的大小約為250 nm至230 nm之間，另一方面，磷前驅物的添加量會影響球狀結構的完整度，添加量太低甚至不含磷前驅物球狀結構將不復存，在電化學分析中，更進一步地發現，鎳金屬與含磷化合物複合材料會比純鎳金屬材料有更好的觸媒活性與交換電流密度，其中以0.2：0.04組成比例為最佳條件，綜合兩項參數電鍍合成之鎳基電觸媒，在1 M KOH的條件下具有高催化產氫活性及穩定性，過電位與交換電流密度分別是173±0.94 mV與-8.22±0.63 μA cm-2。接著再導入奈米碳管，藉由奈米碳管的高導電性與高表面積優點幫助鎳基電觸媒的催化活性，導入奈米碳管後不僅可以影響鎳基電觸媒的型態，球徑大小縮減至200 nm，更可以增加電催化產氫活性，過電位與TOF數值分別是162 mV與367.2 hr-1，TOF數值為沒有導入奈米碳管的1.7倍，意味著觸媒使用效率提升70%。

Nickel-based electrocatalysts were synthesized by electrochemical method. The morphology of electrocatalysts, size and appearance of nanosphere were changed as adjusting the applied current density and composition of electrolyte. The performance of electrochemical hydrogen evolution of nickel-based electrocatalsyts including overpotential, TOF, tafel slope, exchange current density were optimized in terms of the applied current density and the composition of electrolyte. Finally, we imported carbon nanotube into the optimized nickel-based electrocatalysts in order to enhanced the electrochemical performance.

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