In this study, nanoscale PbO₂ was obtained by the hydrolysis reaction of Pb(CH₃COO)₄ in an ethanol solution, and the conventional PbO₂ was prepared by the electrolytic oxidation of PbO powder in a H₂SO₄ solution. The former PbO₂ was identified as single phase β-PbO₂ with the average crystallite size of about 12 nm that had an excellent electrochemical activity, whereas the latter one was a mixture of α-PbO₂, β-PbO₂ and PbSO₄ of about 41 nm average size. A hybrid lead-acid battery cathode consisting of an inner layer of the conventional PbO₂ and an outer layer of the nanoscale PbO₂ was also manufactured. The average diameter of the pores in the hybrid cathode was smaller than that of the conventional cathode of the lead-acid battery, which was made from only the conventional PbO₂. The mass change in the hybrid cathode during the discharge-charge cycle test was relatively high as compared to that of the conventional cathode. Moreover, the cycle tests clearly showed that the reversibility of the discharge-charge reaction was improved in the hybrid cathode since the electrode mass returned to zero even after repeated charge and discharge. As a result, the hybrid cathode was significantly better than the conventional cathode regarding both the current efficiency and the utilization factor of the active materials of the cathode during the discharge-charge reaction. These results may suggest the manufacturing of a novel lead-acid battery with a higher power density and higher capacity.