Iron-cobalt spinel oxide nanoparticles with different Fe/Co ratios have been prepared by the combination of chemical precipitation with simultaneous ultrasonic treatment and subsequent mechanical milling. For comparison, their analogues obtained by thermal synthesis were also studied. Phase composition and structural properties of iron-cobalt oxides are investigated by X-ray diffraction and Moessbauer spectroscopy. Their catalytic behavior in methanol decomposition to CO and methane is tested. A well-defined effect of the preparation method and Fe/Co ratio on the reduction and catalytic properties of iron-cobalt samples is established. (C) 2004 Elsevier B.V. All rights reserved.