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The development of low‐cost, earth‐abundant, and efficient catalysts for overall water splitting, involving the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), attracts tremendous attention in recent years. Herein, this work reports the preparation of Mn‐Co phosphide (Mn‐Co‐P) bifunctional catalysts with a yolk–shell structure by a facile hydrothermal route. The as‐prepared catalysts exhibit an excellent catalytic activity with the low overpotentials of 66 mV at 10 mA cm−2 for HER and 355 mV at 50 mA cm−2 for OER in 1 m KOH, along with an outstanding stability. More importantly, the cell voltage of 1.74 V can achieve a current density of 10 mA cm−2 when assembled as an electrolyzer for overall water splitting. Such superior performance makes the Mn‐Co‐P a promising candidate to replace Pt‐based noble metal catalysts for electrocatalytic applications.

Mn incorporation greatly enhances the electrocatalytic activity of CoP towards both the HER and OER in alkaline solutions.

This work establishes Mn–CoSe2 nanosheets as promising OER electrocatalysts, but also opens an exciting new avenue to enhance their electrocatalytic activity by heteroatom doping.

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