LiCaBO3 :Dy(3+) /Eu(3+) phosphors were synthesized by a solid-state reaction. The synthesized materials were characterized using powder X-ray diffraction pattern (XRD) for confirmation. All the structural parameters were calculated from the XRD data. Scanning electron microscopy (SEM) images showed rod-like morphology. Photoluminescence (PL) emission spectra showed two emissions (484 and 577 nm) in Dy(3+) -doped LiCaBO3 :Dy(3+) phosphors with the concentration quenching effect and the critical distance was calculated to be about 22.76 Å. LiCaBO3 :Eu(3+) phosphor was effectively excited by a near-UV light of 392 nm. The emission spectra exhibited the transition from (5) D0 level to (7) FJ (J = 0-2) with main emission at 614 nm, which comes from the electrodipole transition because of the asymmetric point group. The quenching concentration of Eu(3+) is about 0.2 mol%, and the critical distance was calculated to be about 38.93 Å.