TiO(2) 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 TiO(2) fibers were studied by (1)H nuclear magnetic resonance ((1)H 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 microm 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.