Transition metal oxides with spinel structure have been intensively investigated for energy storage application such as electrochemical supercapcaitors. In the present work, nickel cobalt oxide (NiCo2O4) thin films have been systematically deposited using spray pyrolysis process. Compact and uniform thin films of spinel nickel cobalt oxide with particle size 10–20nm have been obtained by the oxidation of Ni and Co precursors. When evaluated as electrode for supercapacitor, the nanostructured NiCo2O4 thin film deposited at 350°C exhibit the best charge storage property exhibiting high specific capacitance of 752Fg−1 and excellent cycle stability over 1000 cycles. Moreover, nanostructured NiCo2O4 thin film demonstrated high power performance, excellent rate as well as long term cycling stability. The Ragone plots ascertain good power and energy densities for NiCo2O4 thin films. Therefore, NiCo2O4 thin film electrodes are very promising for application in supercapacitors.