Layer of lead sulfate was prepared by anodic oxidation of a lead metal surface under potential 0.0 V vs. mercury sulfate reference electrode. Gradual evolution of a lead sulfate layer during lead oxidation in sulfuric acid environment was investigated by SEM and XRD method. We observed gradual inhibition of the lead sulfate layer during oxidation. Investigation of particle size by the Halder-Wagner analysis method during oxidation revealed a significant increase in particle (crystallite) size mainly during the second part of the oxidation process. The parameters were confirmed by morphology evaluation of images from the scanning electron microscope. Powder XRD device seems to be a useful tool for lead sulfate particle size investigation and measurement of their evolution throughout the lead-acid battery life span.