In this study, a carbon nanocomposite doped with nitrogen-cobalt/nickel oxide (NiCo@NC) derived from a metal-organic framework was synthesized using a controlled pyrolysis method and investigated as an electrode material for supercapacitor applications. The results of structural and morphological analyses including XRD, FTIR, FESEM, TEM, EDX and BET confirmed the successful formation of the NiCo@NC nanocomposite, the preservation of the morphology derived from the initial metal-organic framework and the creation of a porous structure with a specific surface area of ​​21.71 m² g⁻¹ and an average pore diameter of 4.87 nm.
Electrochemical evaluations showed that the NiCo@NC nanocomposite exhibited remarkable supercapacitive performance in alkaline electrolyte medium. Cyclic voltammetry results indicated the dominant quasi-capacitive behavior and the active participation of faradaic reactions in the charge storage process. Galvanostatic charge-discharge test showed that this electrode provides a specific capacity equivalent to F g⁻¹ 553 at a current density of 1 A g⁻¹ and maintains an acceptable capacity of about F g⁻¹ 275 with increasing current density to A g⁻¹ 5. Electrochemical impedance analysis showed a decrease in the charge transfer resistance of the NiCo@NC electrode (Rct ≈ 0.95 Ω) compared to the original metal-organic framework, indicating more efficient electron and ion transport in the nanocomposite structure. Also, the cyclic stability test showed that the prepared electrode retains about 109% of its initial capacity after 1000 charge-discharge cycles. Overall, the results of this study show that the NiCo@NC nanocomposite, due to its high specific capacitance, low charge transfer resistance, and good cyclic stability, is a promising option for the development of advanced electrodes in energy storage systems, especially supercapacitors.