It is reported that we use electrospinning and sol-gel technique to prepare AgCl nanoparticles/PVP nanocomposite microspheres is reported. This is a novel and facile approach. At first, we use sol-gel process to prepare AgCl nanoparticles in the PVP solution, and then the solution is electrospun to obtain AgCl/PVP nanocomposite microspheres. These composites are different from other AgCl-containing materials in the ease of synthesis. We also expect that these composites are applied potentially as antimicrobial materials of medicine and general optic applications. The final products are thoroughly characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and field-emission scanning electron microscopy (FESEM), which shows the formation of AgCl nanoparticles/PVP nanocomposite microspheres. (C) 2008 Elsevier B.V. All rights reserved.