3at. % Eu3+ doped (Y, Gd)2O3 precursor powders with various compositions were synthesized via a sol-gel process, and the precursors were sintered at different temperatures. XRD, FT-IR, Raman and photoluminescence spectroscopy were used to study the phase, microstructure and luminescent properties of the precursors and the sintered powders. The results show that pure (Y, Gd)2O3 polycrystalline phase can be obtained from sintering the precursors at 700°C. The influences of the host compositions on the microstructures and fluorescence properties were analyzed, and the optimized composition was obtained for 3at. % Eu3+ doped (Y, Gd)2O3 powders.