Luminescent one-dimensional nanostructural praseodymium oxyfluoride were first prepared by an economical and simple electrospinning technique in this paper. The formation of one-dimensional nanostructural praseodymium oxyfluoride was carried out by calcining praseodymium trifluoroacetic acid/Poly (vinyl pyrrolidone) [Pr (CF3CO2)(3)/PVP] nanofibers, which were electrospun from the mixture solution of Pr (CF3CO2)(3) and PVP. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) analyses demonstrated the morphology of the one-dimensional nanostructural praseodymium oxyfluoride (PrOF), the structure and the cubic crystal in PrOF. The degradation of polymer and formation of inorganic one-dimensional nanostructural PrOF were characterized by Fourier transform infrared (FT-IR) and Elemental analysis by energy dispersive X-ray (EDX) spectra. The characteristic photoluminescence from one-dimensional nanostructural PrOF were observed with an ultraviolet-light excitation at 306 nm. (c) 2007 Elsevier B.V. All rights reserved.