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Hydrazine (N 2 H 4 ) is considered as one of the most potential energy storage materials in liquid fuel cells, as it contains high energy and power density, and the highefficiency oxidation of N 2 H 4 in fuel cells has drawn great attention. However, the most used catalysts are expensive noble metal catalysts, thus the development of highly efficient non-noble metal catalysts is crucial to reduce the cost of hydrazine oxidation in practical industry. Herein, we synthesized a series of CoFe-layered double hydroxides (CoFe-LDHs) intercalated with different anions via a simple one-step co-precipitation method for the electrooxidation of hydrazine. Through altering the intercalated anions of CoFe-LDHs, the defects and the electronic structure can be well controlled, and the catalytic performance for the electrooxidation of hydrazine were well promoted by using NO 3 À intercalated into CoFe-LDH compared with other anions (like Cl À , BO 3 3À , CO 3 2À ). This work developed a series of hydrazine electrooxidation catalysts and established the relationship between the intercalated anions, the fine structure of the catalyst and the electrocatalytic performance.