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Non-platinum-based critically and rationally fabricated electrocatalysts show promising efficiency in electrochemical oxygen evolution reaction (OER) due to their reliability and costeffectiveness. Herein, a hydrothermally designed oxygen-defective Sm 2 O 3 /Fe 2 O 3 composite with gyroid morphology provides superior active sites with high porosity and mass charge transport in a catalytic system. All of the fabricated materials were characterized via different analytical techniques. The Sm 2 O 3 / Fe 2 O 3 hierarchical composite displays an outstanding lower overpotential (272 mV) to attain a current density of 10 mA/ cm 2 and a lower Tafel slope (75 mV/dec) compared to the individual materials Sm 2 O 3 and Fe 2 O 3 in alkaline media. The remarkable electrocatalytic intrinsic OER performance of oxygendefective Sm 2 O 3 /Fe 2 O 3 is ascribed to the strong synergistic effect among both materials due to their unique gyroid structure, and such architecture exhibits extraordinary electrical properties due to its porous structure. Hierarchical Sm 2 O 3 /Fe 2 O 3 exhibits marvelous activity and stability at an applied potential (0.7 V) with a slight decrease in current density. All of the extraordinary results acquired from electrochemical activity make Sm 2 O 3 /Fe 2 O 3 a promising electrocatalyst for electrochemical energy generation.

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