A new electrode structure based on a three-dimensional mesoporous matrix was developed. Nanoparticles of gamma-iron oxide (Fe2O3) were introduced into the mesopores of a carbon matrix (mesoporous carbon, CMK-3) by oxidizing metallic iron, which was electroplated in the matrix. The resulting structure was found to have a high charge-discharge capacity when used as the positive electrode of a lithium battery. The iron oxide nanoparticles bonded tightly to the electrically conductive electrode framework, and showed a high activity for the electrochemical reaction: Fe2O3 + 6Li -> 3Li(2)O + 2Fe. (C) 2011 Elsevier B.V. All rights reserved.