In this study, neodymia doped poly(vinyl) alcohol/zirconium-cerium acetate (PVA/Zr-Ce) nanofibers were prepared using the electrospinning technique, and then calcined at 800 degrees C for 2 hours. For this purpose, PVA/Zr-Ce polymer solutions doped with different concentrations of neodymia were prepared using electrospinning technique, and then calcined and sintered at 800 degrees C for 2 hours. The effect of neodymia doping was investigated in terms of solution properties, morphological changes and thermal characteristics. The fibers were characterized by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and scanning electron microscope (SEM). The measurements showed that the conductivity, pH, viscosity, and surface tension of the hybrid polymer solutions have decreased with increasing Nd acetate content. The FT-IR spectra of the fibers were in good accordance with the literature. The average crystal size values for calcined and sintered samples which were obtained from precursor solutions were calculated. XRD analysis showed that the crystallite size was decreased with increasing Nd content. This result is verified by the calculation of the total areas of the peaks appeared in the XRD spectra. The very sharp and high intense peaks found in the diffraction patterns revealed the crystalline nature of the product. Moreover, the SEM micrograph of the fibers showed that the average fiber diameters decreased with increasing Nd content.