Samples of Sm and Mg co-doped ceria electrolyte of Ce 1-x Sm x-y Mg y O 2-d (x = 0.2; y = 0.00, 0.05, 0.1, 0.15, and 0.175) were synthesized by sol-gel process. The prepared samples were sintered at 1100 and 1400°C for 4 h. The bulk densities were measured by Archimedes method. XRD measurements indicate that the synthesized samples were in single-phase cubic fluorite structure (space group Fm3m). The cell parameters decrease with the concentration of Mg, and 2h values slightly shift towards right. The particle sizes obtained were between 7.14 and 17.44 nm. The sintered sample achieved 95% of theoretical density. FTIR spectra of samples sintered at 1400°C indicates weak interactions between 3550-3400 cm -1 and 1600-1300 cm -1 are attributed to O-H stretching modes and strong bonds 850-450 cm -1 are assigned to characteristic Ce-O vibrations. The surface morphology and chemical composition were analyzed by SEM and EDS, SEM micrographs show spherical faceted grains, and the samples were crack free, dense material with some pores on surface which are inconsistent with density results. The average grain size obtained was 0.5 lm. Particle size obtained by TEM was in agreement with that obtained by XRD. The high-density ceria co-doped ceramic can be used as electrolyte in SOFC.