Structural characterization of transition metal highly doped carbon aerogels obtained through the sol–gel polymerization process of the formaldehyde with the potassium salt of 2,4-dihydroxybenzoic acid, followed by metal ions exchange using Ni(II) and Cu(II) aqueous solutions, supercritical drying with liquid CO 2 and carbonization at 1050°C under inert atmosphere has been performed. Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy were used and it was found that the metal-containing phase is more homogeneously distributed in Cu-doped carbon aerogels. The presence of the metal species determines both the growth of graphitic nanoribbons and the change of framework of the interconnected carbon particles.