Y 2 O 3 :Eu 3? hollow nanofibers were prepared by calcination of the electrospun PVP/[Y(NO 3 ) 3 ? Eu(NO 3 ) 3 ] composite nanofibers, and then Y 2 O 2 S:Eu 3? hollow nanofibers were successfully synthesized by sulfurization of the as-obtained Y 2 O 3 :Eu 3? hollow nanofibers via a double-crucible method using sulfur powders as sulfur source. The samples were investigated in detail by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy, and fluorescence spectroscopy. XRD analysis shows that the Y 2 O 2 S:Eu 3? hollow nanofibers are pure hexagonal phase with the space group of P " 3m1. SEM observation indicates that as-prepared Y 2 O 2 S:Eu 3? nanofibers are obvious hollowcentered structure with the mean outer diameter of 184 ± 26 nm. Under the excitation of 260-nm ultraviolet light, the Y 2 O 2 S:Eu 3? hollow nanofibers exhibit red emissions of predominant emission peaks at 628 and 618 nm originated from 5 D 0 ? 7 F 2 energy levels transitions of Eu 3? ions. The luminescent intensity of Y 2 O 2 S:Eu 3? hollow nanofibers is remarkably increased with the increase of doping concentration of Eu 3? ions and reaches a maximum at 3 mol % of Eu 3? ions. The emitting colors of the samples are located in the red region in CIE chromaticity coordinates diagram. The possible formation mechanism of Y 2 O 2 S:Eu 3? hollow nanofibers is also proposed. This preparation technique could be applied to prepare other rare earth oxysulfide hollow nanofibers.