Europium-doped yttrium oxide (Y2O3:Eu3+) nanofibers were successfully prepared via an electrospinning method followed by annealing at temperatures up to 1200 degrees C. Mixed solutions of yttrium nitrate, europium nitrate and poly(vinyl pyrrolidone) (PVP) were used as precursors. Poly(vinyl pyrrolidone) polymer was used as a template for obtaining fiber morphology and was then removed during the annealing process to yield Y2O3:Eu3+ fibers. The fibers were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier-transform infrared (FTIR), and photoluminescence (PL) spectrometry. The effect of the heating profile on the morphology, crystallinity, and photoluminescent properties of the nanofibers was systematically investigated. The diameter of the prepared fibers decreased with increasing temperature and a high heating rate caused the polymer to melt quickly and cross-links to form between the fibers. In addition, crystallite size and photoluminescent intensity Of Y2O3:Eu3+ phosphor fibers increased with increasing temperature.