Nanocrystalline ceria-doped-zirconia powder, with the composition Zr 0.80 Ce 0.20 O 2.0 , was synthesized by a combustion technique, using glycine as the fuel and the corresponding metal nitrates as oxidants. This process involves mild conditions, as the external temperature required to initiate the combustion is only ≈250°C. In order to explore the possibility of tailoring the powder properties, different oxidant-to-fuel ratios were used. The products were characterized by XRD to ascertain the phase purity and crystallite size estimation. The crystallite size of the best sample, as also seen by TEM, was found to be in the range of 7–10nm. The surface areas of the fine powders, as obtained from the BET technique, were in the range 17–24m 2 /g. The nature of agglomerates was studied by dynamic light scattering. This nanocrystalline powder, resulted in highly dense pellets, at a relatively lower temperature, which is attributed to the superior powder properties. The sintered microstructure, as studied by SEM, revealed the presence of fine grains. The Small Angle X-Ray Scattering (SAXS) was used to study the fractal behavior and particle size distribution of these nanoparticles. The Raman spectroscopy unambiguously showed the product to be tetragonal.