Tb3+ and Eu3+ ions co-doped containing monoclinic GdPO4 nanocrystals were successfully obtained by a straightforward combustion method. The crystal structure and optical characteristics were investigated by methods: XRD, photoluminescence spectra (PL). The XRD result indicates the GdPO4:10%Tb, x%Eu had monoclinic phase and the average particle size was about 10 nm. Under excitation wavelength at 394 nm, photoluminescent emission spectra of GdPO4:10%Tb, x%Eu nanopowders show strong characteristic emission of Eu3+ ions and no characteristic emission of Tb3+ ions was found. However, under the excitation of 273 nm or 368 nm, the emission spectra of the samples were shown characteristic emission of Tb3+ ions with 5D4 - 7FJ (J=3-6) transitions and Eu3+ ions with 5D0-7FJ (J=0-4) transitions.
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