The special features of nano -structured materials have been motivating the search for new synthesis methods for these types of materials. This paper is concentrated on the characterization of carbon nanostructured materials containing iron ions synthesized by a new method based on the reaction of fine -dispersed Al flakes with dichloroethane in paraffin medium in the presence of iron chloride forming catalytic complexes at different calcined temperatures, and at different gaseous medium. This chemical -based synthesis route is briefly described, and the feasibility of obtaining such systems. Characterization was done by X -ray fluorescence microscopy (XRFM), X -ray diffractometer (XRD), which revealed, respective ly, the presence of oxides and their nanoscale structures, including the elemental distribution and mass thickness of the these elements over the layers . In addition, the surface morphology of these complexes was also conformed by N2 adsorption analyses and scanning electron microscope (SEM).