FexOy-SiO2 nanocomposites were prepared by sol-gel method by using two SiO2 sources and Fe(SO4)(2)center dot 7H(2)O as raw materials. The amorphous gels were thermally treated up to 1000 degrees C. The initial gel and the thermally treated samples were characterized by thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA) and infrared spectroscopy. The presence of hematite was confirmed by the obtained Mossbauer spectra which showed the characteristic sextet. The total amount and the size distributions of the hematite nanoparticles can be controlled via the initial precursors and subsequent by annealing conditions. (C) 2006 Elsevier B.V. All rights reserved.