(Ni+RuO2)/Ni active cathodes were prepared by electrochemical co-deposition of suspended RuO2 particles along with Ni2+ ions onto Ni substrates from an electrolyte solution (Watt bath). Morphology and composition of the cathodes were investigated by SEM and EDX analysis. The observations revealed the RuO 2-Ni layers covered by cauliflower-like particles which distributed homogeneously on the Ni substrate. Particle size and distribution of RuO2 particles in suspension and on the cathode surface were studied by light scattering (LS) and X-ray map techniques, respectively. The LS results revealed a Gaussian distribution with an average RuO2 particle size of 527nm in suspension while X-ray map showed a non-uniform nano particle size distribution below 100 nm. Electrochemical activity of the cathodes were evaluated by linear sweep voltametry (LSV) and the results showed that the enhanced activity of the cathodes were mainly ascribable to the RuO 2 content or the increase in the active sites. The effect of Ni substrates pre-treatment on activity and morphology of prepared cathodes showed morphology changes and enhanced effect on electrochemical activity of the cathodes