The selective reduction in Hz of oxide solid solutions produces nanocomposi
te powders in which transition metal nanoparticles are dispersed inside and
on the surface of the oxide matrix grains. When using a H-2/CH4 reducing a
tmosphere, the metal nanoparticles that form on the surface of the oxide gr
ains act as catalysts for the CH4, decomposition and, because of their smal
l size at high temperatures (>800 degreesC), favor the in-situ nucleation a
nd growth of single-wall and thin multiwall carbon nanotubes. This article
reviews our results on the synthesis and characterization of M-MgAl2O4 (M =
Fe, Fe/Co, Fe/Ni) nanocomposite powders, without and with carbon nanotubes
, emphasizing the information that can be derived from Mossbauer spectrosco
py as a complement to other characterization techniques.