CeO₂ and Gd-doped CeO₂ nanoparticles were synthesized by microwave-assisted method. The structural properties of cerium oxide were analyzed by XRD. The XRD pattern confirmed the cubic structure of cerium oxide. The morphology and size of the CeO₂ and Gd-doped CeO₂ nanoparticles were analyzed by SEM and TEM analysis. From the SEM and TEM images it was confirmed that the pure cerium oxide exhibited the spherical morphology whereas Gd-doped CeO₂ shows rod like morphology as it was confirmed by SEM and TEM images. Raman spectra confirm the F2g mode of vibration of cerium oxide and it was slightly shifted in the Gd-doped cerium oxide sample due to incorporation of Gd.