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Herein, a transition metal dissolution‐oxygen vacancy strategy, based on dissolution of highly oxidized transition metal species in alkaline electrolyte, was suggested to construct a high‐performance amorphous Co(OH)2/WOx (a‐CoW) catalyst for the oxygen evolution reaction (OER). The surface reconstruction of a‐CoW and its evolution were described by regulating oxygen vacancies. With continuous dissolution of W species, oxygen vacancies on the surface were generated rapidly, the surface reconstruction was promoted, and the OER performance was improved significantly. During the surface reconstruction, W species also played a role in electronic modulation for Co. Due to its rapid surface reconstruction, a‐CoW exhibited excellent OER performance in alkaline electrolyte with an overpotential of 208 mV at 10 mA cm−2 and had long‐term stability for at least 120 h. This work shows that the transition metal dissolution‐oxygen vacancy strategy is effective for preparation of high‐performance catalysts.

Herein, vanadium‐doped cobalt carbonate hydroxide, V−CoCH, was synthesized as efficient catalyst for water splitting. Vanadium species were partially dissolved in the early stages of the oxygen‐evolution reaction (OER), inducing self‐etching of the catalyst surface, which is helpful for catalyst surface reconstruction and resulted in a higher number of active sites and oxygen vacancies. The synergy between V‐doping and oxygen vacancies improved the catalytic activity: V−CoCH showed an exceptional OER catalytic performance with an overpotential of 183 mV at 10 mA cm−2. The water‐splitting cell consisting of V−CoCH only required 1.52 V to reach 10 mA cm−2. Theoretical calculations revealed that vanadium in V−CoCH played an important role in electron regulation of active sites. The oxygen vacancies had an important effect on improvement of the OER performance through not only the exposure of more active sites but also through modulation of the electronic structure. This work provides an effective strategy for constructing high‐performance electrocatalysts.

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