A series of NaY(MoO4)2∶Eu3+@SiO2 up-conversion luminescent material were prepared by hydrothermal method. The structure and luminous properties of the samples were analysed by X-ray diffraction(XRD),Scanning electron microscope (SEM), energy spectrometer (EDS), Fourier transform infrared spectrum (FT-IR), fluorescence (FL) spectrum et al. The results indicate that the diffraction peak positions of the SiO2 core-shell structure samples are consistent with standard pattern of NaY(MoO4)2∶Eu3+at characteristic diffraction peaks and no impurity diffraction peaks appear at all. The morphology of NaY(MoO4)2∶Eu3+@SiO2 is a core-shell structure. NaY(MoO4)2∶Eu3+is coated on the surface of SiO2 microspheres.The sub-microparticles of NaY(MoO4)2∶Eu3+@SiO2 is obtained.It can be known that the Y3+lattice positions are taken place by Eu3+from analysis of EDS and XRD; the Si-OH bond in the SiO2 microsphere can band the metal ion together. Under near-infrared light excitation at 793 nm, the NaY(MoO4)2∶Eu3+@SiO2 samples exhibit red emission at 616 nm. The luminescence intensity of NaY(MoO4)2∶Eu3+@6.2SiO2 is about 3 times stronger than NaY (MoO4) 2∶Eu3+.