Pradeep Reddy Vanga

In the present work, Fe‐incorporated bimetallic NiCo–MOF with a microspherical morphology was successfully synthesized via solvothermal route at 170 °C within 6 h. The formation of FeNiCo–MOF framework and the influence of Fe incorporation on its physicochemical properties were systematically investigated using XRD, FTIR, and FESEM. The X‐ray photoelectron spectroscopy (XPS) analysis confirmed the coexistence of multiple oxidation states of Ni, Co, and Fe, while N ₂ adsorption–desorption studies confirmed the presence of a mesoporous framework favorable for electrolyte transport. The electrochemical properties were evaluated in a three‐electrode configuration using 3 M KOH as the electrolyte. The Fe incorporated NiCo–MOF leads to better electrochemical properties and delivered a specific capacity of 449 C g ⁻¹ at 1 A g ⁻¹ , compared to Ni–MOF (220 C g ⁻¹ ) and NiCo–MOF (390 C g ⁻¹ ). The assembled FNCMǁAC asymmetric supercapacitor delivered an energy density of 20.44 Wh kg ⁻¹ at a power density of 800 W kg ⁻¹ . The device retained 76.7% of its initial charge‐storage performance with a coulombic efficiency of 88.5% after 6500 cycles. Notably, an asymmetric prototype device powered a red LED, demonstrating its practical potential. Overall, these findings suggest that Fe incorporation can be utilized to improve the charge‐storage performance of NiCo–MOF‐based electrodes for supercapacitor applications.