Preparation by pyrolysis of aerosols and structural characterization of Fe-doped mullite powders

Amorphous Fe-doped 2SiO(2). 3Al(2)O(3) powders were prepared by pyrolysis o f aerosols generated from solutions of TEOS, AI(III) nitrate, and Fe(III) n itrate in methanol. The study of the thermal evolution of these powders rev ealed that the presence of Fe(III) promotes mullite formation and that thes e cations enter into the mullite lattice at the first stages of crystalliza tion at similar to 900 degrees C. It was also found that the amount of Fe(I II) in solid solution with mullite increased as increasing temperature from 900 to 1400 degrees C. The limit of Fe(III) incorporation into mullite in the as-prepared powders was in the range previously reported for samples pr epared by the ceramic procedure (similar to 11 Fe2O3 wt%). The additional i ron phase appearing in samples with an iron content above this limit consis ted of an iron oxide spinel, which probably contained some AI(III) cations in solid solution. Finally, the analysis of the EXAFS spectra of the heated samples showed that the iron cations incorporated into the mullite lattice are mainly located at octahedral positions. (C) 2000 Elsevier Science Ltd. All rights reserved.