Abstract

Abstract This study proposes a novel approach for the rapid transformation of bimetallic NiCo‐oxides into trimetallic NiCoPt alloys using a pulsed laser technique in an ethanol medium in the presence of Pt salts. The electrochemical results demonstrate the exceptional dual‐functional activity of the optimized NiCoPt‐10 alloy, effectively catalyzing both hydrogen evolution reaction (HER) and hydrazine oxidation reaction (HzOR). Specifically, the NiCoPt‐10 alloy presents a low overpotential of 90 mV at 10 mA·cm −2 for HER and a small working potential of 0.068 V versus the reversible hydrogen electrode (RHE) at 10 mA·cm −2 for HzOR. In situ Raman spectroscopy and theoretical calculations delivered insights into the dual‐functional activity of the NiCoPt alloy. Consequently, the overall hydrazine splitting (OHzS) electrolyzer, employing a NiCoPt‐10||NiCoPt‐10 configuration, required only 0.295 V to deliver 10 mA·cm −2 . Notably, using this dual‐functional NiCoPt‐10 catalyst as the cathode combined with Zn foil as the anode in a Zn–hydrazine (Zn‐Hz) battery, achieved efficient hydrogen (H 2 ) production with an energy efficiency of 97%. Furthermore, self‐powered H 2 production is realized by integrating the Zn‐Hz battery with the OHzS electrolyzer, demonstrating its excellent potential for practical applications. Thus, this rapid synthetic strategy can aid in designing effective electrocatalysts for addressing challenges in H 2 energy production.