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Low‐cost, stable and highly active electrocatalysts for the oxygen evolution reaction (OER) are needed to improve the efficiency of hydrogen production via water splitting. However, developing such a catalyst is still a challenge. Zinc ferrite (ZnFe2O4) is non‐toxic and made from cheap and earth‐abundant materials making it a potential raw material for synthesizing “green” low‐cost catalysts for the OER. However, it has largely been ignored due to its low stability, conductivity and OER‐inactive Zn2+. Herein, ZnFe2O4 is used effectively as a pre‐catalyst to synthesize core‐shell ZnFe2O4@Zn(Fe)OOH polycrystalline heterostructures in situ via cyclic voltammetry. The ZnFe2O4@Zn(Fe)OOH heterostructures display much higher OER catalytic activity and stability than the benchmark RuO2 catalyst in alkaline medium, owing to its high conductivity, stability and electrochemically active surface area (ECSA). Our findings thus reveal a new and effective way by which ZnFe2O4 can be applied in water electrolysis.