beta-NaGdF4: Yb, Tm/beta-NaGdF4: Eu and beta-NaGdE4: Yb, Tm, Eu particles were successfully synthesized by two different methods, solvothermal method and high-energy ball milling. The properties were measured by X-ray diffraction (XRD), TEM and luminescence spectra. All samples shown the strong photoluminescence intensity under 980 nm light excitation and emission of Eu3+ was observed. Finally, two methods are compared in paper.