One of the most challenging targets in oxygen reduction reaction (ORR) electrocatalysts based on N-doped carbon materials is the control of the pore structure and obtaining nanostructured thin films that can easily be incorporated on the current collector. The carbonization of nitrogen-containing polymers and the heat treatment of a mixture of carbon materials and nitrogen precursor are the most common methods for obtaining N-doped carbon materials. However, in this synthetic protocols, the surface area and pore distribution are not controlled. This work enables the preparation of 2D-ordered N-doped carbon materials through the carbonization of 2D polyaniline. For that purpose, aniline has been electropolymerized within the porous structure of two different templates (ordered mesoporous Silica and ordered mesoporous Titania thin films). Thus, aniline has been impregnated into the porous structure and subsequently electropolymerized by means of chronoamperometry at constant potential. The resultant samples were heat-treated at 900 °C with the aim of obtaining 2D N-doped carbon materials within the template structures. Polyaniline and polyaniline-derived carbon materials have been analyzed via XPS and TEM and characterized by electrochemical measurements. It is worth noting that the obtained 2D-ordered mesoporous N-doped carbon materials have proved to be highly active electrocatalysts for the ORR because of the formation of quaternary nitrogen species during the heat treatment.
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