本研究中使用直徑127 μm之白金線作為微陽極，並以銅線作為陰極，搭配微陽極導引電鍍法(Microanode-guided electroplating, MAGE)來製作鎳鎢鋅合金三維微結構。透過改變鍍浴中鋅離子濃度(0.25 mM~2.00mM)與析鍍偏壓(5.3 V~5.9 V)進行電鍍，欲析鍍出具有鎳、鎢、鋅之微結構。其中利用SEM觀察表面形貌、EDS分析化學組成、XRD分析晶體結構，得知微結構之特性，COMSOL模擬電鍍時電場分布。將微結構浸入1.0 M KOH(pH = 14)之鹼性水溶液中，進行電化學產氫效能測試，測試方法有四種，分別為陰極極化曲線、循環伏安法、計時電位法、電化學阻抗圖譜，找出產氫性能最佳之微柱。 採用 Z2鍍浴 以 MAGE製程 設定兩極間距在 50 μm 下 析鍍偏 壓 5.5 V，所析鍍出的 Z2-Ni50W41Zn9微柱產氫效能最佳 ，塔弗斜率-72 mV/dec為最低，並有最大交換電流密度值8.36 mA/cm2，循環伏安第50週次時最大電流密度為-622 mA/cm2，產氫起始過電位最低為-0.16 V，僅需-0.23 V便可使電流固定-300 mA/cm2下，電荷轉移阻抗僅有4.64 Ω∙cm2 得出 鎳鎢鋅 比鎳 鎢合金 有更佳 產氫效能 證實鋅的 添加可改質鎳鎢合金電極。;This study uses platinum wire with a wire diameter of 127 μm as the anode to fabricate three-dimensional microstructures of Ni-W-Zn alloys by Microanode-guided electroplating (MAGE). Change the concentration of ZnSO4·7H2O (0.25 mM ~ 2.00 mM) and bias voltage (5.3 V~5.9 V) are used for electroplating to fabricate Ni-W-Zn microstructures. The surface morphology of microstructure was observed by SEM, EDS analysis of the chemical composition, XRD analysis of crystal structure and COMSOL simulated electric field distribution. Ni-W-Zn microstructures were characterized in 1.0 M KOH via cyclic voltammetry (CV), chronopotentiometry (CP), cathodic polarization, and Electrochemical impedance spectroscopy (EIS), four electric analyses to study their hydrogen reduction to evaluate their catalytic reactivity performance for hydrogen evolution. The Z2 plating bath MAGE process was used with spacing set at 50 μm, and bias voltage was set at 5.5 V. The resulting that Ni54W41Zn5 alloy microcolumn is the best cathode material available for hydrogen production. The Tafel slope was the lowest at -72 mV/dec, exchange current density value of 8.36 mA/cm2, and the current density at the 50th cycle with a maximum value of -622 mA/cm2, and the lowest hydrogen production initial overpotential -0.16 V. When current density was set at -300 mA/cm2, it only need -0.23 V overpotential to obtain. In the EIS measure, the charge-transfer resistance of it is only 4.64 Ω∙cm2, which can produce Ni-W-Zn alloys that are more useful than Ni-W alloys, meaning adding the Zn element could modify Ni-W alloys.
