Nanophosphor with the nominal composition of Ca0.8Zn0.2TiO3∶Pr3+, Na+ (CZTOPN) was synthesized at relatively low temperature by the sol-gel method. Metal ions were dispersed by citric acid in ethylene glycol solvent and then react with Ti(OC4H9)4 to form sol and gel. The decomposition process of the precursor, and crystallization and particle size of CZTOPN were examined by thermal analysis (TG-DSC), powder X-ray diffraction (XRD), and scan election microscopy (SEM). Results of TG-DSC and XRD reveal that the composition of Ca0.8Zn0.2TiO3∶Pr3+, Na+ changes with the sintering temperature. SEM data indicate that the diameter of particles is under 50 nm even if the sintering temperature increases to 1000 ℃. In contrast to a solid state reaction, the excitation spectra of samples synthesized by the sol-gel method shift blue about 10 nm and the emission intensity at 617 nm increases significantly.