Nanofibers of poly(vinyl pyrrolidone) (PVP)/Eu3+, with diameters of 300-900 mn were prepared by using sol-gel processing and electrospinning technique. The products were characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR), and photoluminescence (PL). The results indicated that, Eu3+ was successfully embedded in the one-dimensional hybrid nanofibers, and the PVP/Eu3+ hybrid nanofibers had favorable photoluminescence properties. (c) 2007 Chang Lu Shao. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.