New titanium-substituted vanadium and iron antimonates have been prepa
red with nominal compositions VSb1-xTixO4, V1-xTixSbO4 and FeSb1-xTixO
4, where 0 < x < 1. Conventional solid state reactions between vanadiu
m(V) oxide, antimony(III) oxide and titanium(IV) oxide over 2 days gav
e rutile-related vanadium antimonates of formulation V1-ySb1-yO4, wher
eas materials prepared in 15 min in a microwave oven adopted VSb1-yO4-
2y or VSb1-yO4-3/2y type structures. The structural and reduction prop
erties of the mixed metal antimonates have been examined and found to
be influenced by the method of preparation.