The advanced plasma process of microarc treatment in electrolytes was utilized to prepare oxide layers on aluminum and titanium substrates by anodic conversion. This paper reports results on morphology, structure, growth rates, hardness and water contact angle measurements of titanium and aluminum oxidized surfaces obtained by microarc discharge in ecologically clean and safe electrolytes. Porous oxide layers were formed on the sample surface after the microarc treatment. The morphology of surfaces was dependent on the current intensity during the treatment. The pore diameter in the films decreased with the increase in current intensity and the thickness of the oxide film increased almost linearly with the time of treatment for a constant input power.