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New composite material-multi-walled carbon nanotubes (MWCNTs) coated with thin iron films-have been prepared by MOCVD growth technique using iron pentacarbonyl as the iron source. Their structures and morphologies were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and thermal gravimetric analysis. The NEXAFS C1sand Fe2p-spectra of the composite materials MWCNTs-pyrolytic Fe were studied by total electron yield mode with using synchrotron radiation Russian-Germany beamline at BESSY-II. The study has shown that top layers of the MWCNTs in composite do not have essential destruction, coating of MWCNT's-surface is Fe 3 O 4 and this coating is continuous. The iron oxide adhesion is provided by chemical binding between the carbon atoms of the MWCNT's top layer and the oxygen atoms of the coating.