| 摘要: | 本研究採用微陽極導引電鍍(Micro-anode Guided Electroplating , MAGE)法成功製備三維鎳-鉬合金微柱，並於含有奈米碳管與二硫化鉬奈米顆粒之合金鍍液中進行複合電鍍，以開發具備 1T-MoS₂/CNT 異質結構鑲嵌於 Ni-Mo 合金之複合微柱材料。其中所使用之 1T 相 MoS₂/CNTs 為本研究先行以水熱合成法製備而得。
所製備之 Ni-Mo 合金微柱與 1T-MoS₂@CNTs/Ni-Mo 複合微柱，分別經由掃描式電子顯微鏡（SEM）觀察其表面形貌，透過能量散射光譜儀（EDS）進行元素組成分析，並以 X 光繞射儀（XRD）鑑定其晶體結構。後續將此等微柱作為工作電極，浸入 1.0 M KOH 電解液中進行析氫反應(hydrogen evolution reaction, HER)電催化效能之系統性評估，測試方法包括線性掃描伏安法（LSV）、循環伏安法（CV）、雙電層電容法以評估電化學活性表面積（ECSA）、計時電位法（CP）與電化學阻抗分析（EIS）等。實驗結果顯示，在成分為Ni 佔 34 at. %、Mo 佔 47.4 at. % C 佔 15.5 at. % S佔 3.1 at. %的條件下，所得複合微柱展現最佳之產氫性能，其塔弗斜率（Tafel slope）為 50 mV/dec，電流密度達 -10 mA/cm² 時所需過電位（η₁₀）僅為 -50 mV，最大陰極電流密度1236 (-mA/cm2) (50th cycle)，且電荷轉移阻抗（Rct）低至 3.77 Ω·cm²，顯示其在 HER 過程中具備快速電子轉移能力與優異的電催化活性。綜合以上分析結果，可證實二硫化鉬@奈米碳管與鎳-鉬合金之共鍍設計可有效提升催化表面活性位點數量並促進界面電荷轉移速率，進而增進複合電極於鹼性水溶液中之產氫效能，顯示本研究所開發之微結構複合材料於未來氫能轉換技術中具備高度應用潛力。
;In this study, three-dimensional nickel–molybdenum (Ni-Mo) alloy micropillars were successfully fabricated using the Micro-anode Guided Electroplating (MAGE) technique. Composite electrodeposition was conducted in a plating bath containing carbon nanotubes (CNTs) and molybdenum disulfide (MoS₂) nanoparticles, aiming to develop Ni-Mo composite micropillars embedded with a 1T-MoS₂/CNT heterostructure. The 1T-phase MoS₂/CNT composite used in the process was synthesized in advance via hydrothermal synthesis.
The as-deposited Ni-Mo alloy and 1T-MoS₂/CNTs/Ni-Mo composite micropillars were characterized by scanning electron microscopy (SEM) for surface morphology, energy-dispersive X-ray spectroscopy (EDS) for elemental composition, and X-ray diffraction (XRD) for crystalline structure. These micropillars were further used as working electrodes for hydrogen evolution reaction (HER) measurements in 1.0 M KOH electrolyte. The electrochemical performance was evaluated through linear sweep voltammetry (LSV), cyclic voltammetry (CV), electrochemical surface area (ECSA) determination, chronopotentiometry (CP), and electrochemical impedance spectroscopy (EIS).
The experimental results revealed that the composite micropillar with a composition of 34.0 at. % Ni, and 47.4 at. % Mo, 15.5 at. % C, 3.1 at. % S exhibited the best HER performance, including a low Tafel slope of 50 mV/dec, an overpotential (η₁₀) of -50 mV at -10 mA/cm², a maximum cathodic current density 1236 (-mA/cm2) (50th cycle) , and a low charge transfer resistance (Rct) of 3.77 Ω·cm². These results indicate high catalytic efficiency and favorable charge transfer characteristics during the HER process.
In summary, the co-deposition of MoS₂@CNTs with Ni-Mo alloy significantly enhances the number of active sites and accelerates interfacial charge transfer, thereby improving the electrocatalytic HER performance. The developed composite micropillar structure demonstrates great potential for future hydrogen energy applications. |
