Silicoaluminate substrates doped with Dy at different concentrations are synthesized by high temperature solid state method. X-ray diffraction phase analysis shows that one of the main phases is Dy3Al2(AlO4)3. By Raman spectroscopy analysis, the intensity of the Raman peak is at 874.5 cm-1, which is related to the stretching vibration of Dy-［AlO4］. With the increase of Dy doping content, the intensity of Raman peaks increases first and then decreases. The peak at 419.9 cm-1 is related to the bending vibration of Dy-［AlO4］. With the increase of Dy doping content, the intensity of Raman vibration peak, the peaks of fluorescence spectrum measured by fluorescence spectrophotometer and the photoluminescence spectrum measured by Raman spectrophotometer all show the rule of first increasing and then decreasing. The matching amount of Dy-［AlO4］ increases gradually, and when the amount of Dy doping exceeds a certain limit, concentration quenching occurs in the system, which results in the decrease of fluorescence properties. Compared with Tb system, the Raman spectra of the two systems have great similarities and slight differences. The Raman vibration peaks of Tb doped materials are 870.0 and 408.0 cm-1. The fluorescence intensity of two kinds of fluorescent materials doped with different elements are consistent, which indicates that the matching amount of rare earth elements with Al (Si) oxygen tetrahedron is the key factor to determine the fluorescence properties of the materials.