Redox Promoted Rapid and Deep Reconstruction of Defect‐Rich Nickel Precatalysts for Efficient Water Oxidation

Abstract Understanding the reconstruction mechanism to rationally design cost‐effective electrocatalysts for oxygen evolution reaction (OER) is still challenging. Herein, a defect‐rich NiMoO 4 precatalyst is used to explore its OER activity and reconstruction mechanism. In situ generated oxygen vacancies, distorted lattices, and edge dislocations expedite the deep reconstruction of NiMoO 4 to form polycrystalline Ni (oxy)hydroxides for alkaline oxygen evolution. It only needs ≈230 and ≈285 mV to reach 10 and 100 mA cm −2 , respectively. The reconstruction boosted by the redox of Ni is confirmed experimentally by sectionalized cyclic voltammetry activations at different specified potential ranges combined with ex situ characterization techniques. Subsequently, the reconstruction route is presented based on the acid‐base electronic theory. Accordingly, the dominant contribution of the adsorbate evolution mechanism to reconstruction during oxygen evolution is revealed. This work develops a novel route to synthesize defect‐rich materials and provides new tactics to investigate the reconstruction.