Metallic nanostructures have attracted the interest of researchers due to their fundamental importance and potential applications in nanodevices, sensors and catalysts. Co-AAO nanocomposites were obtained by using a sol-gel method that uses ultrasonic vibrations to induce the penetration of a colloidal solution through the pores of an anodized aluminum oxide (AAO) template. The AAO template, with the sol into its pores, was annealed at 648 K. The entire dip-anneal-dip�process was repeated three times. Finally, the metal nanostructures were formed by further annealing at 873 K in hydrogen atmosphere for 1 h. The morphology and structure of Co-AAO were investigated by using SEM, HRTEM, XRD and EPR methods.