A cyclic voltammetric (CV) technique was used to study the combined effects of annealing temperature and time on the pseudocapacitance of thermally treated electroprecipitated nickel hydroxide thin films. Through the analysis of the areas of the CVs cycled between 0 and 0.35V (versus Ag/AgCl) it is shown that the optimal treatment condition for maximum film capacitance occurs at 300°C for 3h. On the other hand, using the anodic and cathodic peak currents of the CVs cycled between 0 and 0.5V (versus Ag/AgCl), the maximum film capacitance is also shown to occur at a thermal treatment condition of 300°C and 3.5h (or 320°C and 3.2h for linear approximations). The two methods demonstrate simple ways of extracting useful information on the electrochemical performance properties of thin films.