Red Gd 2 O 3 :Eu nanophosphors were prepared by novel sucrose-assisted combustion method. The sucrose hydrolysis and complexing procedures were discussed by the Fourier transform infrared spectroscopy (FTIR) analysis. The effect of sucrose-to-metal ratio (S:M) on morphology and luminescence intensity of Gd 2 O 3 :Eu nanocrystals were investigated. And the optimum ratio was found to be S:M=7:1, as confirmed by the results of scanning electron microscope (SEM), transmission electron microscope (TEM) and photoluminescence (PL) measurements. The highest photoluminescence emission from the particles obtained at S:M=7:1 was about 85% of the commercial red phosphors.