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Carbon aerogels and Cr-, Fe-, Co-, and Ni-containing carbon aerogels were obtained by pyrolysis, at temperatures between 500 and 1800 °C, of the corresponding aerogels prepared by the sol−gel method from polymerization of resorcinol with formaldehyde. All samples were characterized by mercury porosimetry, nitrogen adsorption, X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), and Raman spectroscopy. Results obtained show that carbon aerogels are, essentially, macroporous materials that maintain large pore volumes even after pyrolysis at 1800 °C. For pyrolysis at temperatures higher than 1000 °C, the presence of the transition metals produced graphitized areas with three-dimensional stacking order, as shown by HRTEM, XRD, and Raman spectroscopy. HRTEM also showed that the metal−carbon containing aerogels were formed by polyhedral structures. Cr and Fe seem to be the best catalysts for graphitization of carbon aerogels.

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