Nanoparticulate films of NiO and carbon are fabricated by electrospray coating of respective aqueous precursors on Ni foam. The adhesion of the active layers to the substrate during solvent evaporation, calcination, or carbonization is demonstrated for both types of electrodes. The effect of metal precursor composition and calcination temperature is analyzed through X-ray diffraction (XRD), scanning electron microscopy (SEM), and electrochemical techniques. The capacitance of NiO and carbon film electrodes is found to be 343 mF cm(-2) (286 F g(-1)) and 118 mF cm(-2) (118 F g(-1)), respectively at a current density of 1 mA cm(-2). The supercapacitor in an asymmetric setup delivers specific energy and specific power to the levels of 12.6 Wh kg(-1) and 1.7 kW kg(-1) respectively, with the capacitance retention of 88% after 2000 cycles at 5 mA cm(-2).