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ABSTRACT Heterostructures show great potential on highly efficient electrocatalysts for oxygen evolution reaction (OER) owing to optimization of electronic structure, synergies, exposure to multiple active sites. In present work, we establish a spherical nanoflower‐structured nickel‐iron carbonate hydroxides/silicate hydroxides (denoted as NiFeCH/SH) with crystalline/amorphous heterostructure by a facile hydrothermal synthesis strategy. Characterization analysis confirms the controlled partial phase conversion without structural collapse, which is based on the Ni‐Fe bi‐metallic effect. The heterostructures under bimetallic effect provides the optimized catalyst with good electrical conductivity and abundant active sites, which makes it achieve exceptional OER performance with an ultralow overpotential of 251 mV at 10 mA cm −2 and a small Tafel slope of 31.8 mV dec −1 , alongside outstanding long‐term stability. The enhanced stability is originated from the protection of silicate. Density functional theory (DFT) methods reveal that the enhanced activity stems from moderate electronic structure caused by suppressing electron transition to e g orbitals of metal active sites. This work establishes a dual‐regulation strategy integrating tetrahedral silicate engineering and bimetallic cooperation to simultaneously enhance OER activity and durability, offering new perspectives for designing robust alkaline water electrolysis catalysts through electronic and defect structure manipulation.
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