The structural and morphology of copper-stabilized zirconia samples prepared by sol–gel techniques in different calcination time and temperature are reported. This research work has been proposed and verified that the calcination temperature and time strongly influenced the morphology as well as interaction between the active species and the support. The results obtained from the laboratory test indicate that cubic ZrO2 and copper oxide are present in the structure if the calcination temperature is under 400°C. Cubic ZrO2, tetragonal ZrO2 with small amount of monoclinic ZrO2, and CuO are formed after calcination at 500°C. Heating under 500°C will result in amorphous compounds being formed, suggesting that 500°C could be a phase transition point. The effect of calcination time is investigated by morphology and structural changes of CuO–ZrO2 at 600°C during 2, 3.5, 5.5, 7.5, and 10 h. Incorporation of copper in ZrO2 lattice results in a loss of order in the ZrO2 structure when it is calcined. A further increase in the temperature of calcination leads to the phase changes in ZrO2 structure.