NiCo2O4 (NCO) nanostructures were synthesized by a simple hydrothermal method using three different surfactants such as ethylene glycol (EG), oxalic acid (OA) and ammonium fluoride (NHF). Morphology of the different nanostructured materials has been recorded using SEM. The electrochemical performance of the material has been demonstrated using three electrode system. NCO-EG urchin-like nanostructure exhibits the highest specific capacitance of 416 F g−1 at a current density of 0.5 A g−1 and it evolves 73.3 % of capacitance retention at 10 A g−1.NiCo2O4 (NCO) nanostructures were synthesized by a simple hydrothermal method using three different surfactants such as ethylene glycol (EG), oxalic acid (OA) and ammonium fluoride (NHF). Morphology of the different nanostructured materials has been recorded using SEM. The electrochemical performance of the material has been demonstrated using three electrode system. NCO-EG urchin-like nanostructure exhibits the highest specific capacitance of 416 F g−1 at a current density of 0.5 A g−1 and it evolves 73.3 % of capacitance retention at 10 A g−1.