NaYF4:Yb3+/Tb3+and NaYF4:Yb3+/Tm3+double doping fluoride nanomaterials with different doping concentrations were prepared by hydrothermal synthesis. In these materials, the Yb3+ was used as sensitizer to assist in luminous, Tb3+ and Tm3+ were added to the matrix sodium yttrium fluoride as activators of luminous center. The morphology and luminous properties of NaYF4:Yb3+/Tb3+ and NaYF4:Yb3+/Tm3+ nanoparticles were investigated by scanning electron microscope (SEM), X-ray diffraction andfluorescence spectrum. The X-ray diffraction patterns of the series of samples well match the NaYF4 standard card. Upconversion luminescence spectra of materials under 980 nm laser excitation were obtained and the mechanism was also analyzed. Excited by 980 nm laser, the emission spectra of NaYF4:Yb3+/Tb3+ including blue, green and red light, which correspond to the radiative transition of 5D4→7F6, 5D4→7F5, 5D4→7F1, respectively. The strong 480 nm emission can be seen in NaYF4:Yb3+/Tm3+ excited by 980 nm laser, corresponding to the electron transition energy band of 1G4→3H6. A strong red light emission band centered at 660 nm is corresponding to the 1G4→3F4 energy level transition. © 2020, Science Press. All right reserved.