Reducing energy consumption and improving energy utilization efficiency has become the focus of research in the 21st century. Electrocatalytic water splitting is one of the promising strategies for producing hydrogen energy. In this study, the non‐noble nickel‐iron layered double hydroxide (NiFe‐LDH) catalyst is deposited on the electrochemically intercalated graphite/graphene (G/GE) substrate and directly used as the self‐supported and binder‐free electrode for electrocatalytic water oxidation. The Ni2Fe1‐LDH@G/GE catalyst shows a low overpotential of 194 mV at a current density of 10 mA cm–2, which is better than the noble metal catalyst IrO2 (314 mV) and RuO2 (330 mV) and many other related works. This research provides a facile way to directly prepare the catalyst electrode with high performance and low cost.

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