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A novel nonprecious Fe2O3 nanoparticle decorated NiO nanosheet (Fe2O3 NPs@NiO NSs) composite has been obtained by a rapid one-pot electrochemical exfoliation method and can be used as an efficient oxygen evolution reaction (OER) catalyst. In the nanocomposite, the Fe2O3 NPs are uniformly anchored on the ultrathin graphene-like NiO nanosheets. At the same time, we also studied the influence of the Fe/Ni molar ratio on the morphology and catalytic activity. The Fe2O3 NPs@NiO NSs nanocomposite possessed a high BET surface area (194.1 m2