The development of cost‐effective electrocatalysts is a key issue to promote the practical application of hydrazine as a viable energy carrier. Herein, a nickel‐foam‐supported Ni−Zn alloy catalyst is synthesized by electrodeposition and anodic dissolution methods. The developed catalyst with an opennanowall network structure and robust adhesion exhibits high activity and good durability for electrooxidation of hydrazine in an alkaline medium. For example, a current density of 300 mA cm−2at 0.40 Vand an onset potential of −0.15 V vs. the reversible hydrogen electrode are achieved in a 0.10 M hydrazine and 1.0 M NaOH solution at 30 °C. Phase and structure analysis by XRD, SEM, and XPS is conducted to gain insight into the excellent catalytic performance of theNi−Zn alloy catalyst. Such an understanding is of particular importance in the design of efficient non‐precious catalysts.
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