A MOF‐Derived CoFe ₂ O ₄ /NiS ₂ Hierarchical Electrode on Carbon Cloth for Efficient Overall Water Splitting

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Developing efficient and robust electrocatalysts for the hydrogen evolution reaction (HER) is essential for advancing water‐splitting technologies. Herein, we synthesized the CoFe 2 O 4 /NiS 2 ‐MOF/CC (carbon cloth) composite by first growing a Co‐MOF scaffold in situ on carbon cloth (CC) to form a three‐dimensional (3D) porous scaffold, which was then subjected to a one‐step hydrothermal sulfurization for anchoring CoFe 2 O 4 and NiS 2 . The 3D Co‐MOF/CC scaffold affords a high specific surface area and open porosity, exposing abundant active sites and significantly enhancing HER electrocatalysis. Under hydrothermal sulfurization at 180°C and an Fe:Ni molar ratio of 1:1, the resulting 3D catalyst delivers excellent HER and OER activity in 1 M KOH, with low overpotentials of 94 mV at 10 mA·cm −2 for HER and 291 mV at 50 mA·cm −2 for OER. It also delivers stable overall water splitting for 22 h at a cell voltage of 1.58 V at 10 mA·cm −2 , showing competitive performance among recently reported MOF‐based and MOF‐derived electrocatalysts. Hence, this work demonstrates a cost‐effective route to high‐performance, bifunctional catalysts for overall water splitting.