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The application of heteroatom doped cobalt (Ni@Co/C) prepared from a porous metal–organic framework as the cathode material for the rechargeable zinc–air batteries has been demonstrated. The Ni@Co/C‐modified electrode showed an excellent catalytic activity toward oxidation–reduction reaction and oxygen evolution reactions. The Co/C catalysts, which were Co particle impregnated on graphitic carbon powders, were synthesized after the calcination of Co3 (SDA)3(DMF)2 precursor, and then Ni deposition (Ni@Co/C) was followed on it by chemical reduction. Linear sweep voltammetry measurement indicates that Ni@Co/C‐H800, which had Ni particles on Co/C derived from MOF at 800 °C under N2, exhibited excellent performance. The stable charging/discharging profiles at 20 mA cm−2 of current were obtained for the 350 h in alkaline medium, suggesting Ni@Co/C‐H800 as a potential candidate for oxidation–reduction and evolution reactions.

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