A Mo-doped organic aerogel and its corresponding carbonized derivative at 1000 degrees C were obtained. Both samples were treated in a H(2)/Ar flow. After this treatment, a mixture of Mo(VI) and Mo(2)C was detected in both samples. The results obtained indicate that the presence of H(2) in the gas flow is necessary to obtain the carbide phase, due to the formation of CH(4) or even CH(x)() species that reduce and carburize the molybdenum oxide phase. Carburization of the Mo-doped organic aerogel yielded better results compared with carburization of the Mo-doped carbon aerogel.