The CaWO4:Ln(3+)@SiO2(Ln=Tb, Dy and Ho) nanoparticles were synthesized via a combustion process at 800 C, using citric acid as chelating agent and fuel, ammonium nitrate as fuel, boric acid as flux material and silica as supports. The persistent phosphor nanoparticles were characterized by X-ray diffraction (XRD), reflectance UV-vis and fluorescence spectroscopy (PL) and transmission electron microscopy (TEM) techniques. XRD patterns indicated that crystalline calcium tungstate with scheelite structure was produced. The reflectance UV-vis spectra showed the broad absorption band of WC:11 groups and the PL spectra showed the WO42- wide excitation band, broad emission band of WO42- and characteristic emissions of Ln(3+) ions. The average particle sizes were determined by TEM, which are about 50 nm. (C) 2010 Elsevier B.V. All rights reserved.