The synthesis of active electrocatalyst materials for the water-splitting reaction, which requires suitable intrinsic and surface properties, is an essential strategy in the field of renewable energy. In this work, a Ni–Mn–P@Co–S nanostructured electrocatalyst was synthesized using a two-step hydrothermal-electrodeposition method to reduce the hydrogen evolution reaction (HER) overpotential. In the first step, Co–S microwires were synthesized using a hydrothermal method. Subsequently, Ni–Mn–P nanosheets were formed on them via cyclic voltammetry (CV) with varying scan rates and cycle numbers. The results indicated that the sample synthesized at a scan rate of 5 mV s−1 and 10 cycles exhibited η10 and η100 values of 89 mV and 256 mV, respectively. Additionally, the electrochemical stability of this sample was found to be 88.5% in the galvanostatic test. This study introduces a novel, cost-effective and efficient method for synthesizing electrode materials for energy conversion and storage systems.

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