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Fe‐doped Ni (oxy)hydroxide shows intriguing activity toward oxygen evolution reaction (OER) in alkaline solution, yet it remains challenging to further boost its performance. In this work, a ferric/molybdate (Fe3+/MoO42−) co‐doping strategy is reported to promote the OER activity of Ni oxyhydroxide. The reinforced Fe/Mo‐doped Ni oxyhydroxide catalyst supported by nickel foam (p‐NiFeMo/NF) is synthesized via a unique oxygen plasma etching‐electrochemical doping route, in which precursor Ni(OH)2 nanosheets are first etched by oxygen plasma to form defect‐rich amorphous nanosheets, followed by electrochemical cycling to trigger simultaneously Fe3+/MoO42− co‐doping and phase transition. This p‐NiFeMo/NF catalyst requires an overpotential of only 274 mV to reach 100 mA cm−2 in alkaline media, exhibiting significantly enhanced OER activity compared to NiFe layered double hydroxide (LDH) catalyst and other analogs. Its activity does not fade even after 72 h uninterrupted operation. In situ Raman analysis reveals that the intercalation of MoO42− is able to prevent the over‐oxidation of NiOOH matrix from β to γ phase, thus keeping the Fe‐doped NiOOH at the most active state.

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