Using tetra-n-butyl titanate and magnesium nitrate as raw materials, Dy3+ and Pr3+ ions in the matrix of magnesium titanate (MgTiO3) was successfully synthesized by a modified solid-state reaction. The mixtures to achieve a solid-state reaction were heated in porcelain crucibles at 600 A degrees C for 2 h, 900 A degrees C for 6 h, and 1000.0 A degrees C for 2 h. The reaction products obtained in an air atmosphere were characterized by X-ray powder diffractions. The optimization of reaction conditions were carried out by thermal gravimetry and differential thermal analysis methods. Surface and elemental analyses were performed by using on SEM instrument. The excitation and emission spectra were recorded by photoluminescence spectrophotometer.