Nanomaterials La2O3:Sm3+was prepared by combustion synthesis. The morphology and structure were characterized and analyzed by TEM and XRD. The luminescent properties were also investigated. The results were indicated that the mean particle size of La2O3:Sm3+ nanomaterials with hexagonal structure were approximately 34 nm. Because of the Sm3+ doping, the position of diffraction peaks of La2O3:Sm3+ moved to the right slightly; It was observed that intrinsic excitation band of Sm3+ was located in around 411 nm; Under the 411 nm excitation, the major emission peaks at 4G5/2 → 6H5/2 (568 nm)，4G5/2 → 6H7/2 (611 nm, the highest intensity) and 4G5/2 → 6H9/2 (654 nm) were observed. The emission spectrum indicated the location of the Sm3+ ions were asymmetric. The decay lifetime of the Sm3+ ions was about 202 μs; The chromaticity coordinate was approximately (0.5849, 0.4143).