The mechanical milling of alpha-Fe2O3 or V2O5 with Sb2O3 results in the formation of small particle FeSbO4 or VSbO4. Milling also induces the conversion of cubic Sb2O3 to the orthorhombic modification and the transformation of alpha-Sb2O4 to beta-Sb2O4. The milling-induced alpha- to beta-Sb2O4 phase transition is even more facile in the presence of vanadium or iron. (C) 2004 Kluwer Academic Publishers.