Red phosphor (Y, Gd)BO3:Eu3+ with grain shape, small size, non-agglomerate, high crystallinity and good photoluminescence (PL) intensity was prepared by a complex method that the precursor of the phosphor was prepared by co-precipitation method and the phosphor was prepared by combustion method. The SEM photos and the photoluminescence spectrum excited under VUV show that the morphology and luminescent properties of this phosphor are satisfied when an appropriate amount of urea was adopted as the combustion agent in the preparation procedure.