本研究以泡沫鎳（NF）為基材製備Ni-Fe LDH電極，並透過Co參雜、乙二醇輔助層間距調控及Ni-Fe LDH二次披覆三種策略，探討其結構調控機制與水分解催化性能。結果顯示適量Co參雜可在維持LDH層狀結構下，調整Ni、Fe、Co金屬中心的電子環境，改善反應中間物吸附與界面電荷傳輸。其中Ni-Fe-Co 0.4 LDH@NF表現最佳，其OER與HER過電位分別為220 mV與188 mV；然而Co含量過高易造成片層堆疊與團聚，使有效活性位點利用率下降。乙二醇輔助水熱法可使LDH層間距由7.59 Å增加至約9.3–9.6 Å，理論上有利於電解液滲入及離子傳輸，但同時可能降低層板排列規則性與結晶性，因此層間距擴張並未直接轉化為更佳的電化學性能。經Ni-Fe LDH二次披覆後，表面形成片狀結構，可增加反應界面並改善電荷傳輸，其中Co參雜量為0.3 g、披覆時間為200 s之03200樣品，在HER中具有最低過電位178 mV。
於雙電極整體水分解測試中，03200電極僅需1.63 V即可達到10 mA cm⁻²，相較於Pt/C∥IrO₂電極的1.64 V，操作電壓降低約0.61%，產氫電壓效率提升約0.67%，理論產氫能耗降低約0.62%，顯示二次披覆可有效改善整體水分解效率並降低產氫能耗。

This study fabricated Ni–Fe layered double hydroxide (LDH) electrodes on nickel foam (NF) and investigated three modification strategies: Co doping, ethylene-glycol assisted interlayer expansion, and secondary Ni–Fe LDH coating.Appropriate Co doping preserved the LDH structure while regulating the electronic environments of Ni, Fe, and Co centers, thereby improving intermediate adsorption and interfacial charge transfer. Ni-Fe–Co 0.4 LDH@NF showed the best catalytic performance, with OER and HER overpotentials of 220 and 188 mV, respectively. Excessive Co doping caused nanosheet stacking and agglomeration, reducing the utilization of active sites.
Ethylene glycol increased the LDH interlayer spacing from 7.59 Å to approximately 9.3–9.6 Å, which could promote electrolyte penetration and ion transport. However, the enlarged spacing also reduced structural regularity and crystallinity, preventing further electrochemical improvement. After secondary Ni–Fe LDH coating, sheet-like and wrinkled structures were formed, increasing the reaction interface and enhancing charge transfer. The 03200 sample exhibited the lowest HER overpotential of 178 mV.
For overall water splitting, the 03200∥03200 electrolyzer required only 1.63 V to reach 10 mA cm⁻², slightly lower than the 1.64 V required by Pt/C∥IrO₂. The operating voltage and theoretical hydrogen-production energy consumption were reduced by approximately 0.61% and 0.62%, respectively. These results demonstrate that Co doping and secondary LDH coating effectively enhance bifunctional electrocatalytic performance.

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