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In this present research, we synthesized pure α‐Fe2O3, NiO, and a microporous α‐Fe2O3@NiO heterostructure electrode via the spray pyrolysis method. The microporous α‐Fe2O3@NiO heterostructure electrode, with its highly porous structure, offers a larger electrode‐electrolyte interface, which results in improved electrochemical performance. Specifically, the microporous heterostructure exhibited a higher specific capacitance of 530.87 F/g at a current density of 7 mA/cm2 in a 1 M NaOH electrolyte, as compared to α‐Fe2O3 (187.12 F/g at 7 mA/cm2) and NiO (492.69 F/g at 7 mA/cm2). The microporous α‐Fe2O3@NiO heterostructures exhibited significantly enhanced electrochemical performance as compared to the individual α‐Fe2O3 and NiO samples, owing to the synergistic effect of the heterostructure. Furthermore, the microporous α‐Fe2O3@NiO heterostructure exhibited high specific capacitances and exceptional cycling stability for more than 2000 cycles, indicating their potential as excellent electrode for supercapacitor devices. [ABSTRACT FROM AUTHOR]