The synthesis of electrocatalysts which used simultaneously as electrodes for the hydrazine oxidation reaction (HzOR), and hydrogen evolution reaction (HER) can significantly improve the efficiency of hydrogen production in the water splitting process. Here, Ni–Co–Fe–P binder-free nanosheets were fabricated using the electrochemical deposition method and used as an effective, stable, and cost-effective electrode for hydrazine-assisted electrochemical hydrogen production. Taking advantage of high surface area, being binder-free, and synergistic effect between the elements in the electrode composition, this electrode showed unique electrocatalytic activity and stability. When this electrode was used as a bifunctional electrode for HzOR-HER, a cell voltage of 94 mV was required to reach a current density of 10 mA cm−2. The results of this study indicated that the Ni–Co–Fe–P electrode is an excellent candidate for the hydrogen production industry.

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