The compound lead (IV) oxide ï¢-PbO2was prepared in our laboratory. The Thermal behavior of this compound was studied using both techniques of Thermogravimetery and Differential Scanning Calorimetery under O2 gas atmosphere from 25 to 600°C. The identityof products at different stages were confirmed by XRD technique. Results obtained using both techniques support same decomposition stages for this compound. Three distinct energy changes takes place, two endothermic and one exothermic in DSC results. The amount of ïH for each peak is reported.