Leitao Xu, Yelin Yao, Wenjie Wu, Wei Chen, Cairong Wang, Yandong Wu, Zhonghuan Zhu, Zhuoran Lu, Ta Thi Thuy Nga, Chung‐Li Dong, Yuqin Zou, Shuangyin Wang
Abstract The synthesis of hydrazine from the electrooxidation of ammonia (NH 3 ) presents a promising pathway, yet it is hindered by the strong thermodynamic preference for the oxidation of hydrazine. Here, we describe an electrochemistry‐mediated strategy that reverses the thermodynamic order during NH 3 oxidation, enabling sustainable hydrazine production. This process utilizes cyclohexanone (C 6 H 10 O), derived from the electrooxidation of cyclohexanol (C 6 H 11 OH), as a mediator to prevent the over‐oxidation of NH 3 . The in situ generation of cyclohexanone (C 6 H 10 O) at the catalyst interface effectively prevents the over‐oxidation of NH 3 , while cation effect accelerates NH 3 capture during the reaction. Furthermore, the developed manganese (Mn) doped nickel hydroxide electrocatalyst (Mn‐Ni(OH) 2 ) not only improves NH 3 tolerance of the catalyst but also promotes the conversion of nitrogen‐containing intermediates. This scalable approach achieves gram‐scale production at a constant current of 800 mA, offering economic advantages over industrial methods, paving the way for a sustainable transformation of the chemical industry.