The structure of binary iron-cobalt oxide nanosystems-precursors of bimetallic catalysts-is studied by Mössbauer spectroscopy, X ray diffraction, and small angle X ray scattering. The oxide system under study represents a promising material for creating new metallic nanocatalysts for ammonia synthesis. The structural evolution in the composition range 100Fe/0Co-5Fe/95Co is found to correspond to the tran sition from fine grained α Fe 2 O 3 to mixed iron-cobalt spinels of various compositions and degrees of dis persity.