In this study, rare earth ions Yb3+ and Er3+ co-doped into NaMgF3∶Gd3+ nanoparticles were successfully prepared by modified solvothermal method. The structure of the prepared sample was determined by X-Ray Diffraction, and the average particle size was calculated by using the Debye-Scherrer formula. The particle size of the sample was within the nanometer range. The results of further experiments show that with the change of the concentration of Gd3+ in the reactants, the morphology of the nanoparticles appears to change from nanosheets to nanowires, so as to realize the regulation of nanocrystals. At the same time, the photoluminescence properties of the prepared nanoparticles under 980 nm excitation light were studied in detail. It is worth noting that the emission intensity of nanoparticles gradually increases with the change of Gd3+ doping concentration, and the tendency of green to red emission occurs.