Eu 3+ activated CaSiO 3 , (Ca, Ba) SiO 3 and (Ca, Sr) SiO 3 have been prepared by sol-gel technique. Residual solvent and organic contents in the gel were removed by firing at 100°C for 3-4 h at 300 and 600°C for 2 h. Small exothermic shoulder around 850 to 875°C, as observed in DTA curve, corresponds to crystallization temperature of the doped calcium silicate. Influence of firing temperature on the luminescence of Eu 3+ shows the maximum emission intensity in gel fired at 850°C. Photoluminescence emission peak is observed at 614 nm due to 5 D 0 → → 7 F 2 transition of Eu 3+ ion in (Ca, Ba) SiO 3 and (Ca, Sr) SiO 3 phosphors, when excited by 254 nm. The (Ca, Ba) SiO 3 material is proposed as an efficient red phosphor.