NaGd(MoO4)2∶xEu3+(x=10%, 20%, 30%, 40%) and NaGd(MoO4)2∶7%Eu3+, ySO2-4/BO3-3 phosphors were prepared by hydrothermal method with sodium citrate as a surfactant. The crystal phase, morphology and luminescent properties of the prepared samples were characterized. The results showed that the structures of NaGd(MoO4)2∶xEu3+ and NaGd(MoO4)2∶7% Eu3+, ySO2-4/BO3-3 phosphors were tetragonal scheelite. The characteristic absorption peak of SO2-4/BO3-3 was found by infrared spectroscopy, indicating that SO2-4/BO3-3 was successfully incorporated into the matrix. The emission spectrum of NaGd(MoO4)2∶30%Eu3+ was the strongest. Besides, by studying the emission spectrum of NaGd(MoO4)2∶7%Eu3+, ySO2-4/BO3-3 phosphors, it can find that appropriate doping of SO2-4/BO3-3 can enhance the characteristic emission intensity of Eu3+. The addition of 10% SO2-4 or 10% BO3-3 can reduce the doping of Eu3+ by about 3%, which can save the doping amount of rare earth.