Nanoscale Y2O3:Eu phosphors have been prepared by glycine-nitrate solution combustion synthesis. The particle size of resultant powders is much related to the combustion flame temperature, which can be controlled by adjusting the glycine-to-nitrate ratio. The IR spectra, the excitation and the diffuse reflection spectra show the particle-size dependence of optical properties. The quenching concentration of nanostructured phosphors is increased greatly, compared with phosphors synthesized by conventional synthesis method.