The structural properties of annealed nickel oxide and its composites with activated carbon (synthesized via simple precipitation methods) have been addressed using X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen adsorption/desorption method and scanning electron microscopy. The charge storage properties of materials have also been investigated in three- and two-electrode configurations by means of cyclic voltammetry and galvanostatic charging/discharging in alkaline media. The results are consistent with the view that, depending on a method of preparation, the resulting nickel oxide films may exhibit redox characteristics different from that typically observed for nickel oxide-based materials. It is demonstrated that faradaic-type (redox) reactions, that are typical for battery-like materials, contribute predominantly to the high electrode capacity of 257Cg−1 (at 0.1Ag−1). By combining nickel oxide with a capacitive material such as activated carbon within the two-electrode symmetric cell, systems with increased charge-storage capabilities have been obtained. The fact, that the voltage window of nickel oxide-based cell has been broadened positively from 0.6V to 1V upon introduction of activated carbon, has also resulted in the increase of the cell’s energy and power densities as well.