本研究以相對低溫之化學浴法，結合短時間之磷化熱處理方式，在泡沫鎳基板上合成鎳鈷磷硫化物作為產氫及氧化5-羥甲基糠醛(HMF)之雙功能電觸媒電極。為避免HMF在強鹼環境中嚴重的降解情形，本研究在0.1 M KOH電解液中電催化產氫反應(HER)與氧化HMF反應(HMFOR)。在三極式系統中，優化之鎳鈷磷硫電極在1.52 V vs RHE之下催化10 mM 之HMFOR，結果顯示三小時後之HMF轉化率為99.03%，而2,5-呋喃二甲酸(FDCA)之選擇率為92.51%，法拉第效率為95.19%。另外，鎳鈷磷硫電極生成氫氣之法拉第效率為98.5%，並於12小時內維持99.99%之穩定性。本研究進一步在二極式系統中，以鎳鈷磷硫電極進行同步產氫與氧化HMF之電催化反應。以HMFOR取代OER之結果顯示，當電流密度達10 mA cm-2時，所需施加之電壓顯著降低了165 mV。另外，在二極式系統中定電壓(2.12 V)催化5 mM 之HMFOR， 結果顯示78分鐘後之HMF轉化率為95.01%，而FDCA之選擇率與法拉第效率分別為84.32%與87.11%，而生成氫氣之法拉第效率為96.07%。本研究成功地利用非貴金屬電觸媒電極，同步生產高附加價值之化學品FDCA和乾淨的能源H¬2，提升電催化產氫之經濟效益。

In this study, a relatively low-temperature chemical bath combined with phosphating heat treatment was used to synthesize nickel-cobalt phosphorus sulfide on nickel foam as an electrocatalyst for hydrogen evolution reaction (HER) and 5-hydroxymethylfurfural oxidation reaction (HMFOR). To avoid the severe degradation of HMF, this study performed electrocatalytic HER and HMFOR in 0.1 M KOH. In a three-electrode system, the optimized electrode catalyzed 10 mM HMFOR at 1.52 V vs RHE, and the HMF conversion was 99.03%, while the selectivity of 2,5-furandicarboxylic acid (FDCA) is 92.51%, and the Faraday efficiency (FE) is 95.19%. In addition, the FE of HER is 98.5%, and it maintains a stability of 99.99% within 12 hours. In the two-electrode system, the optimized electrode was used to catalyze HER and HMFOR. The results of replacing OER with 5 mM HMF HMFOR showed that when current density reached 10 mA cm-2, the cell voltage was reduced by 165 mV. Furthermore, the results of catalyzing a 5 mM HMFOR at 2.12 V showed that the conversion of HMF was 95.01%, while the selectivity and FE of FDCA were 84.32% and 87.11%, respectively. Also, The FE of HER is 96.07%. In this study, non-precious electrocatalyst were used to simultaneously produce FDCA and H2, improving the economic benefits of electrocatalytic hydrogen production.

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