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Oxidizing vacancies in nitrogen‐doped carbon have recently been reported to enhance the oxygen reaction activity of air cathodes, but their specific role has remained elusive and controversial. Herein, the critical role of oxidizing the vacancies in enhancing the oxygen reduction reaction for metal–air battery is identified with density functional theory. Deliberate introduction of oxygen‐enriched vacancies in nitrogen‐doped carbon is shown experimentally to provide superior oxygen reduction activity. In situ X‐ray powder diffraction gives direct observation of the oxygen reactions in a zinc–air battery catalyzed by vacancy‐enriched oxidized carbon; the intensity changes of the carbon peak show continuous chemisorption of oxygen intermediates on the carbon cathode during discharge. The air‐cathode performance is shown to exceed that with Pt/C+IrO2 catalysts.
Oxidizing vacancies in nitrogen‐doped carbon are theoretically and experimentally confirmed to greatly improve the oxygen reduction activity of an air cathode. The facilitated adsorption of oxygen intermediates on the air cathode during zinc–air battery operation is directly observed by in situ X‐ray powder diffraction and the robust battery reversibility is verified by in situ Raman spectroscopy.