Submicron scale composite fibers of SiO2/TiO2 with various compositions have been prepared by electrospinning a sol-gel precursor of tetraethyl orthosilicate(TEOS) and titanium(IV) isopropoxide(TiP), followed by calcination. Any gelator or binder has not been used in this direct preparation process for composite fibers, and the maximum amount of titania for suitable fiber formation was about 50 mol%. The sintered composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FT-IR) spectroscopy. Our results show that the surface morphology and crystallization behavior of electrospun fibers are largely influenced by the calcination temperature and the content of TiO2. XRD results also reveal that the anatase phase in composite fibers can be preserved even after high temperature processing at lower content (x=0.1, 0.2) of titania. (c) 2006 Elsevier B.V All rights reserved.