This work deals with the evolution of a mechanical mixture of Fe2(MoO4
)3 and alpha-Sb2O4 (prepared separately) during calcination in air at
500-degrees-C over a period of six days. The samples were studied by X
-ray diffraction, X-ray photoelectron spectroscopy, BET surface area,
CTEM, analytical electron microscopy and selected area electron diffra
ction. A reaction occurs between the two phases, leading to a mixture
of Fe2 (MoO4)3, Sb2O4, FeSbO4 and MoO3 with a significant increase of
the surface area. Taking into account previous results, the present wo
rk suggests that the ability of alpha-Sb2O4 to produce oxygen spillove
r facilitates the oxidation of Sb3+ to Sb5+ allowing the solid state t
ransformation to FeSbO4 to take place.