| 摘要: | 本研究首先以實驗室研發的微陽極導引電鍍法(Micro-anode guided electroplating，MAGE) 來製備鎳銅鉬(Ni-Cu-Mo)合金微柱，並測量其在鹼性環境下陰極析氫的效能，並在後續另外利用水熱法來合成1T相二硫化鉬(1T-MoS2)粉末，並將合成出的1T相二硫化鉬粉末加入先前最佳配方之鎳銅鉬合金微柱鍍液中，並同樣利用微陽極導引電鍍法製備鎳銅鉬/二硫化鉬(Ni-Cu-Mo/1T-MoS2)微柱，來比較兩者的效能差異。
而所製備的鎳銅鉬合金微柱與鎳銅鉬/二硫化鉬微柱會分別進行微柱特分析與微柱效能分析，使用掃描式電子顯微鏡(SEM)觀察表面形貌、能量色散X射線光譜(EDX)進行表面成分分析，以及利用X射線繞射(XRD)與穿透式電子顯微鏡(TEM)進行晶體結構鑑定分析。而微柱效能分析則包括線性掃描伏安法(LSV)、循環伏安法(CV)、計時電位法(CP)、電化學活性表面積(ECSA)與電化學阻抗頻譜(EIS)等電化學測試。
研究結果顯示，添加1T-MoS2所製備的複合微柱，其HER效能顯著優於合金微柱。當複合微柱之最佳成分約為Ni 33 at.%、Mo 24.9 at.%、Cu 29.8 at.%、S 12.3 at.% 時，其表面呈現具高表面積的類多孔海綿狀結構。此複合微柱展現了最佳的電化學析氫性能：塔弗斜率(Tafel slope)僅為42.5 mV/dec；在10 mA/cm2的電流密度下，僅需37 mV 的過電位(ƞ10)；陰極峰值電流密度來到1932 mA/cm2；且電荷轉移電阻(Rct)低至 1.87 Ω∙cm2。
這些結果證實了Ni-Cu-Mo/1T-MoS2複合微柱在鹼性環境下具有卓越的析氫能力。本研究認為，1T-MoS2的引入促使微柱形成奈米晶結構，大幅增加了電化學活性表面積 (ECSA)；並且金屬特性的1T相MoS2提供了豐富的反應活性位點。二者協同作用故顯著提升了HER效能，為高效、低成本的氫氣生產提供了具潛力的電催化劑。
;In this study, Nickel-Copper-Molybdenum (Ni-Cu-Mo) alloy micropillars were first fabricated using a lab-developed Micro-anode guided electroplating (MAGE) method, and their cathodic hydrogen evolution reaction (HER) performance in an alkaline environment was evaluated. Subsequently, 1T-phase Molybdenum Disulfide (1T-MoS2) powder was synthesized via a hydrothermal method. This synthesized 1T-MoS2 powder was then added to the previously optimized Ni-Cu-Mo alloy plating bath, and Ni-Cu-Mo/1T-MoS2composite micropillars were fabricated using the same MAGE technique to compare the performance differences between the two.Both the prepared Ni-Cu-Mo alloy and Ni-Cu-Mo/1T-MoS2 composite micropillars underwent comprehensive material characterization and electrochemical performance analysis. Characterization involved scanning electron microscopy (SEM) to observe surface morphology, energy-dispersive X-ray spectroscopy (EDX) for surface composition analysis, and X-ray diffraction (XRD) and transmission electron microscopy (TEM) for crystal structure identification. The electrochemical performance was evaluated through linear sweep voltammetry (LSV), cyclic voltammetry (CV), chronopotentiometry (CP), electrochemical active surface area (ECSA) assessment, and electrochemical impedance spectroscopy (EIS).The results reveal that the composite micropillars prepared with the addition of 1T-MoS2exhibited significantly superior HER performance compared to the alloy micropillars. The optimal composite, with a composition of approximately Ni 33 at.%, Mo 24.9 at.%, Cu 29.8 at.%, and S 12.3 at.%, displayed a high-surface-area, porous, sponge-like morphology. This composite micropillar demonstrated exceptional electrochemical HER performance: a Tafel slope of only 42.5 mV/dec, an overpotential (ƞ10) of just 37 mV required to achieve a current density of 10 mA/cm², a cathodic peak current density reaching 1932 mA/cm2, and a low charge transfer resistance (Rct) of 1.87 Ω∙cm2.These results confirm the outstanding HER capability of the Ni-Cu-Mo/1T-MoS2 composite micropillars in alkaline media. This study suggests that the incorporation of 1T-MoS2 promotes the formation of a nanocrystalline structure, thereby significantly increasing the electrochemical active surface area (ECSA). Moreover, the metallic 1T-phase MoS2 provides abundant reactive active sites. The synergistic effect of these factors leads to a remarkable enhancement in HER performance, presenting a promising electrocatalyst for high-efficiency, low-cost hydrogen production. |
