Electrospinning of a sol-gel and polymer mixture is used to produce titania-alumina (TiO2-Al2O3) fibers with diameters ranging from 200 to 800 nm. These composite metal-oxide fibers were calcined at various temperatures and their morphology is studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The decrease in the average diameter of the fibers with increasing temperature is observed. Powder X-ray diffraction (XRD) reveals that up to 800 degrees C the composite fibers have anatase titania structure whereas at 900 degrees C the fibers exhibit mixture of anatase and rutile phases. It is found that specific surface area decreases as a function of temperature in the 700 -900 degrees C range. The change in phase (anatase-to-rutile) and the increase in crystallite size occur simultaneously. The presence of smaller amount of amorphous alumina in the primarily titania-based structure seems to play the role in stabilizing the anatase phase. (C) 2011 Elsevier B. V. All rights reserved.