The synthesis of a carbon film by the acid-catalyzed polymerization and resinification of furfuryl alcohol with a diluted solution of HCl is studied by combining micro-FTIR and micro-Raman spectroscopies. The detailed study of the evolution of spectra as a function of dosage of furfuryl alcohol and temperature shows that neutral and protonated species are formed at 80 degrees C, while upon gradually increasing the temperature up to 600 degrees C, the viscous polyfurfuryl alcohol resin is transformed into a carbon phase, containing a heterogeneous distribution of pores, with a size in the 100-2000 nm range, as shown by SEM and AFM analyses.