TiO2 precursor fibers were prepared with a new facile polyorganotitanium precursor by a dry-spinning method. The synthesis process. structure of the precursor, and its evolution from the precursor to polycrystalline TiO2 fibers were studied by H-1 nuclear magnetic resonance (H-1 NMR), Fourier transformation infrared (FTIR). X-ray diffraction (XRD), and differential scanning calorimetry and thermal gravimetry analysis (DSC/TGA). The average diameter of the fibers is in the range of 10-20 mu m from scanning electron microscopy (SEM) and the length can reach tens of centimeters. The BET surface area of the fibers calcined at 500 degrees C/2 h is around 160.3 m(2)/g and decreases with temperature increase. (C) 2009 Elsevier Inc. All rights reserved.