Nanocomposites with core/shell structure composed of hematite (alpha-Fe2O3), polypyrrole (PPy) and silver have been successfully synthesized with a three-step reaction process. First, semispherical cores of alpha-Fe2O3 were prepared by the forced hydrolysis of FeCl3. Next, pyrrole was polymerized in the suspension of alpha-Fe2O3 and then composite carrier with alpha-Fe2O3 as core and PPy as shell was produced. Last, a surface reduction-oxidation was carried out between PPy and silver nitrate so as to produce alpha-Fe2O3/PPy/Ag nanocomposites. The as-prepared nanoparticles were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and cyclic voltammogram (CV), furthermore, the effects of reaction conditions on the morphology of nanocomposites were studied in detail. The alpha-Fe2O3/PPy/Ag nanocomposites exhibit excellent electrochemical activity and chemical catalytic properties in the reduction reaction of m-nitrobenzene sulfonic sodium (m-NBS) at room temperature. To our knowledge, the alpha-Fe2O3/PPy/Ag nanocomposites have not been reported. (C) 2012 Elsevier B.V. All rights reserved.