A series of Eu3+, Tb3+, Tm3+ singly and triply doped Ca3Bi(PO4)3 (CBP) phosphors were synthesized by solid-state reaction. Their structure and photoluminescence (PL) properties were first investigated in detail. Rietveld refinement analysis confirmed that the CBP has a cubic unit cell. Its space group was determined to be I3d with cell parameters a = b = c = 9.941 Å and Z = 4. In addition, the Ca3Bi(PO4)3 shows both cation disorder and oxygen sublattice disorder. For the CBP:Eu3+ phosphor, the charge transfer bands in the PLE spectra were different at 293 K and 4.3 K, and a model was presented to give a possible explanation for this phenomenon. CBP:Eu3+ shows intense red emission due to 5D0–7F2 transition and its integral emission intensity and quantum efficiency are higher than the commercial Y2O3:Eu3+ phosphor under irradiation of 397 nm, indicating that the CBP:Eu3+ phosphor might have potential application in the NUV range for solid-state lighting. The CBP:Tb3+ and CBP:Tm3+ phosphors show intense green and blue emission due to 5D4–7F2 transition of the Tb3+ ions and the 1D2–3F4 transition of the Tm3+ ions, respectively. The energy transfer from the Tb3+ to Eu3+ ions was also validated by the spectra and decay curves of the Tb3+ ions. Tunable emission colors were obtained by triply doping Eu3+, Tb3+ and Tm3+ activators in a single host and adjusting their relative ratio.
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