PbO
2 powders, which are the positive active materials in the lead-acid battery, were mechanically milled with Sb
2O
3 powders. It is well known that Sb contained in the grid of lead-acid battery is useful for the protection of the premature capacity loss. Before milling, most of PbO
2 powders consist of tetragonal β-phase, but in the progress of milling process, they were transformed to orthorhombic α-phase. The intensity of X-ray diffraction peaks of Sb
2O
3 decreases with increasing milling time, and after the milling of 5 hours, they almost disappear, which indicates that the alloying between PbO
2 and Sb
2O
3 proceeds during milling process. The intensity of the reduction peak in the cyclic voltammetry (CV) curve of the electrode constructed from the PbO
2 powders is larger than that of the electrode constructed from PbO
2 powders added with Sb
2O
3. The discharge capacity of the electrode constructed from PbO
2 powders increases with increasing milling time, but that of the electrode constructed from PbO
2 powders added with Sb
2O
3 is rather reduced. The difference of the properties between these two electrodes may be ascribed to the difference of the microscopic structure of PbSO
4 particles, which are formed during the discharging process.
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