A series of self-assembled 3D flower-like NaY1-x(WO4)2∶xSm3+(x=0, 0.005, 0.010, 0.015, 0.020, 0.025, 0.030) powders were prepared by hydrothermal method and high temperature sintering, with trisodium citrate as the anchoring agent. The phase structure, morphology, composition and luminescence properties were characterized by X-ray powder diffraction(XRD), scanning electron microscopy(SEM), infrared spectrum(FT-IR) and photoluminescence spectroscopy (PL), respectively. The results show that the synthesized samples are pure NaY(WO4)2 with tetragoonal scheelite structure. NaY(WO4)2∶Sm3+ powders can be excited by a wavelength of 405 nm and exhibit a strong orange-red emission at 600 nm, corresponding to the 4G5/2→6H7/2 magnetic dipole transition of Sm3+. The optimum doping molar fraction of Sm3+ is determined to be of 0.015 based on the maximum intensity of fluorescence emission.