Fe-2O_ 3 /Al-2O_ 3 nanocomposites prepared by using the sol-gel technique were reduced in H-2 atmosphere at different temperatures, and the corresponding Fe/Al_2O_3 nanocomposites were obtained after the reduction of Fe-2O_ 3 /Al-2O_ 3 nanocomposites at 1173 K. The structures and properties of the specimens were studied by X-ray diffraction(XRD), Mssbauer spectroscopy(MS), and vibrating sample magnetometry(VSM). The results show that the reduction temperature has a significant influence on the structure, the grain size, and the magnetic properties of the specimens. Fe - 2O_3 / Al - 2O_3 nanocomposites prepared by using the sol-gel technique were reduced in H -2 atmosphere at different temperatures, and the corresponding Fe / Al_2O_3 nanocomposites were obtained after the reduction of Fe -2O_3 / Al - 2O_3 nanocomposites at 1173 K. The structures and properties of the specimens were studied by X-ray diffraction (XRD), Mssssbauer spectroscopy (MS), and vibrating sample magnetometry (VSM). The results show that the reduction temperature has a significant influence on the structure, the grain size, and the magnetic properties of the specimens.