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The impact of different calcination temperature (550ºC, 650ºC, 750ºC and 850ºC) on the structural/electrical properties of sintered Cu/Sm co-doped CeO2 prepared by sol-gel combustion were studied. The structural property was studied by X-ray diffraction (XRD) and Raman spectroscopy and ultraviolet visible(Uv-vis). The composition and chemical state of Sm/Cu and Ce and electrical conductivity of sintered sample were investigated by X-rays photoelectron spectroscopy (XPS) and electrical impedance spectroscopy (EIS), respectively. XRD pattern showed that all samples have a cubic fluorite structure. Moreover, XRD revealed that the crystallite size and crystallinity increased with the increasing calcination temperature. However, the lattice parameter and oxygen vacancy slightly decreased with the increasing temperature, which indicates the change of oxidation state between Ce4+and Ce3+ . The high conductivity were obtained for samples calcined at 750ºC.
