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Composites of mesoporous alumina and Fe- or Co-containing ferromagnetic nanoparticles have been prepared from appropriate aqueous metal chloride solutions by a sol-gel process. The synthesis products were heat-treated at different temperatures in air or vacuum and then characterized by a variety of techniques. The results indicate that the mesoporous structure of the nanostructured composites has a large specific surface area, a narrow, unior bimodal pore size distribution, and high thermal stability. The phase composition of the magnetic particles in the X-ray amorphous oxide matrix strongly depends on the heat-treatment conditions.