This paper reports the electrochemical synthesis of nickel oxide (NiO) onto a substrate template of anodized-brass (Cu-Zn). Structurally and morphologically all the electrodes, i.e. pristine, anodized and NiO-covered Cu-Zn electrodes, are different from one another. NiO-covered Cu-Zn electrodes were annealed at different temperatures (300-600 °C at 100 °C intervals) and appear suitable for electrochemical supercapacitors; a wide potential range (0.1-0.6 V) and optimum specific capacitance (91.43 F g) are obtained for 400 °C in 0.5 M NaOH electrolyte at 2 mV s scan rate.