The optimal formulation and processing conditions were investigated for the preparation of the phosphorescent ceramic pigment BaAl 1.7 B 0.3 O 4 doped with Eu 2+ and Dy 3+ using the polymeric precursor method or Pechini method. The properties of the synthesized pigment were analyzed by X-ray diffraction, excitation by ultraviolet light, Raman spectroscopy, photoluminescence, and luminescence decay. The hexagonal barium aluminate phase BaAl 2 O 4 could be identified in all doped compounds. The photoluminescence spectra analysis indicated that phosphorescence efficiency increased with higher Eu 2+ concentrations, and that the pigments emitted green light in the visible range of 430–500nm corresponding to the 4f 6 –5d →4f 7 of Eu 2+ transition with curves of luminescence decay between 160 and 790s. We conclude that these techniques and analyses are suitable to produce a high quality phosphorescent pigment suitable for use in the ceramic industry.