Prepared the Er3+/Yb3+ co-doped CeO2 nanocrystalline sparkle powder with the self-propagating high-temperature synthesis, and controlled the particle size of synthesized samples by changing the proportion of rare earth nitrates and glycine. Detected the powder through XRD and SEM, analyzed its microstructure and morphology, and investigated the characteristics of up-conversion luminescence for the sample stimulated by 980 nm laser. The results show that the effect of sample crystallization at annealing temperature 1 000 ℃ is best when the nG/nN equals 0.36 and the grain size is about 50 nm; the effect of up-conversion luminescence performance is best when doping 3% Er3+. When the amount of substance concentration of Yb3+ is 10% and the amount of Er3+is 3%, the effect of up-conversion luminescence performance of the obtained CeO2:Yb3+/Er3+ is best. When stimulates CeO2 substrate with 980 nm excitation light source, the observed up-conversion luminescience peaks are located at 525,545,557,654 and 674 nm, and the band at 525 nm is attributed to the electronic transition 2H11/2→4I15/2, the bands at 545 and 557 nm attributed to the transition 4S3/2→4I15/2, and the bands at 654 and 674 nm to transition 4F9/2→4I15/2.