The phosphor Y2SiO5:Ce3+ was prepared by a sol-gel method and the particle growth process was investigated by XRD, SEM and TEM. After heating at 400 °C, the as-dried gel became a powder composed of mixed phases of polycrystalline Y2O3 and amorphous SiO2. With an increase in temperature, the crystallinity of Y2O3 improved. The sample quickly changed to the pure Y2SiO5 phase when it was heated at 1400 °C for 10 min. SEM indicated that the as-dried gel consisted of large porous particles. At an annealing temperature of higher than 400 °C, the pores in the large particles gradually expanded and grains started to appear. Consequently, the large particles disintegrated into small particles. When the sample was heated at 1400 °C, we obtained fine phosphor particles (around 2 μm) with smooth surfaces. The optimized condition for the preparation of the Y2SiO5:Ce3+ phosphor was to heat at 1400 °C for 2 h. The phosphor Y2SiO5: Ce3 + was prepared by a sol-gel method and the particle growth process was investigated by XRD, SEM and TEM. After heating at 400 ° C, the as-dried gel became a powder composed of mixed phases of polycrystalline Y2O3 and amorphous SiO2. With an increase in temperature, the crystallinity of Y2O3 improved. The sample quickly changed to the pure Y2SiO5 phase when it was heated at 1400 ° C for 10 min. SEM indicated that the as-dried gel consisted of large porous particles. At an annealing temperature of higher than 400 ° C, the pores in the large particles gradually expanded and grains started to appear. (around 2 μm) with smooth surfaces. The optimized condition for the preparation of the Y2SiO5: Ce3 + phosphor was to heat at 1400 ° C for 2 h.