This study explores the synthesis of ultrathin flower architecture of spinel-structured Co3O4 electrodes, on nickel foam using a double hydrothermal method, followed by annealing at 250 °C for 4 h. We systematically investigate the effects of varying reaction times and additional Co2+ treatment during the second hydrothermal process on the morphology and electrochemical properties of Co3O4. Field emission scanning electron microscopy (FE-SEM) images confirm the formation of self-supported hierarchical flowers, characterized by sharp, spike-like nanowires (16–33 nm in diameter) arranged radially. The self-supported optimized hierarchical Co3O4 thin film, characterized by its unique architecture and substantial mass loading of 4.6 mg cm−2, achieved an impressive specific capacitance of 749.48F g−1 at a scan rate of 10 mV s−1 (specific capacity of 182.16 mAh g−1) in 2 M KOH electrolyte and retained 64 % of its initial capacitance after 5000 cycles. Furthermore, a symmetric device demonstrated the ability to illuminate a red LED for approximately 120 s when two devices were connected in series.
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