Novel ZrO2/Al2O3 nanofibers with the average diameter of around 110 nm are fabricated by heat treatment of electrospun zirconium oxychloride (ZrOCl2)/aluminium nitrate (Al(NO3)(3))/polyvinylpyrrolidone (PVP) composite fibers at temperature of 1200 degrees C. Intermediate and the final ceramic filaments are characterized by thermogravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscopy (SEM), energy-dispersive X-rayspectroscopy (EDS) and X-ray diffractometry (XRD). The ZrO2/Al2O3 nanofibers contain mainly tetragonal zirconium dioxide in contrast to pure ZrO2 nanofibers consisting of monoclinic zirconia. It is revealed that Al2O3 impedes the ZrO2 grain growth and stabilizes the tetragonal phase of zirconia forming Al2O3-ZrO2 s olid solution. Fabricated zirconia nanoscale filaments with varying phase composition can be considered, for instance, as promising one-dimensional high-temperature supports for heterogeneous catalysts with controlled activity and selectivity.