Polyvinyl pyrrolidone and polyvinyl alcohol thickeners and Sm(NO3)(3) have been directly processed by electrospinning method to obtain composite nanofibers. Scanning electron microscopy micrographs indicated that the surface of the prepared composite fibers was smooth. X-ray diffraction analysis revealed that the composite nanofibers were amorphous in structure. Sm2O3 nanoparticles and nanofibers were fabricated by calcination of the composite fibers.