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The transition metal-based catalysts have excellent electrochemical oxygen evolution reaction catalytic activity in alkaline electrolytes, attracting a significant number of researchers’ attention. Herein, we used two-step hydrothermal and solvothermal methods to prepare a Ni(OH)₂/MoS₂/NF electrocatalyst. The electrocatalyst displayed outstanding OER activity in 1.0 M KOH electrolyte with lower overpotential (296 mV at 50 mA·cm⁻²) and remarkable durability. Comprehensive analysis shows that reinforcement of the catalytic function is due to the synergistic effect between Ni(OH)₂ and MoS₂, which can provide more highly active sites for the catalyst. This also provides a reliable strategy for the application of heterogeneous interface engineering in energy catalysis.