One-dimensional (Y, Gd)BO3:Eu3+ nanofibers with hexagonal structure have been prepared as potential red phosphors by an electrospinning technique, and characterized with Xray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, differential thermal analysis and photoluminescence spectra. The effect of annealing temperature on the crystallization and luminescence properties has been studied. The main emission position is centered at 591 nm (D-5(0)-F-7(1)). Photoluminescence spectra indicate that higher temperature would result in improved fluorescence capability.