In this paper, a two-step synthesis method for preparing Eu3+ ion-doped Y2O3@YOF core-shell nanocrystals is introduced. Eu3+ ion-doped Y2O3@YOF core-shell nanocrystals were prepared by combining an autocombustion process with a low temperature solid state reaction. X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), photoluminescence (PL) and fluorescence decay were employed to characterize the prepared samples. The results of XRD, TEM and EDS indicated that the products prepared by this method were not a mixture of Y2O3:Eu3+ and YOF:Eu3+ nanocrystals, but Eu3+ ion-doped Y2O3@YOF core-shell nanocrystals. Compared with Y2O3:Eu3+ nanocrystals, a 20% increment in luminescence intensity was observed in the Eu3+ ion-doped Y2O3@YOF core-shell nanocrystals, thus suggesting that coating with a YOF:Eu3+-shell can efficiently block the nonradiative relaxation channels that are induced by surface defect states.