Transition metal oxide nanocrystalline materials are playing major role in energy storage application in this scenario. Nickel oxide is one of the best antiferromagnetic materials which is used as electrodes in energy storage devices such as, fuel cells, batteries, electrochemical capacitors, etc. In this research work, nickel oxide nanoparticles were synthesized by combustion route in presence of organic fuels such as, glycine, glucose and and urea. The prepared nickel oxide nanoparticles were calcined at 600 o C for 3 h to get phase pure materials. The calcined nanoparticles were preliminarily characterized by XRD, particle size analysis, SEM and EDAX. To prepare nickel oxide electrode materials for application in supercapacitors, the calcined NiO nanoparticles were mixed with di-methyl-acetamide and few drops of nafion solution for 12 to 16 h. The above slurry was coated in the graphite sheet and dried at 50 o C for 2 to 4 h in a hot air oven to remove organic solvent. The dried sample was subjected to electrochemical studies, such as cyclic voltammetry, AC impedance analysis and chrono-coulometry studies in KOH electrolyte medium. From the above studies, it was found that nickel oxide nanoparticles prepared by combustion synthesis using glucose as a fuel exhibited resulted in low particle diameter (42.23 nm). All the nickel oxide electrodes have shown better good capacitance values suitable for electrochemical capacitor applications.