Nanocrystalline solid solution CeO2-Nd2O3 powders were prepared by low temperature combustion process.Special attention was paid to the influence of the glycine/metal ratio and calcination temperature on the powders phase structure, morphology and particle size.TG-DSC curves and XRD peaks of different glycine/metal ratio show that smaller particle size can be obtained with a slightly fuel-deficient ratio.XRD results indicate that the as-prepared powders are crystallized in a single fluorite structure.The crystalline size ranges from 9 to 24 nm, which increases with the increase of calcination temperature.The lower SEM images were characterized by the spongy and form-like microstructure of the powders.Organic agent may be gradually eliminated by high temperature calcination process.