A new low temperature synthetic route to binary and ternary metal antimonides is reported. Binary transition metal antimonides prepared include CoSb 3 , CoSb 2 , CoSb, NiSb, NiSb 2 , Cu 2 Sb and Mo 3 Sb 7 ; new ternary compositions prepared include the series Co 1−x Ni x Sb (0.1≤x≤0.9). The intermetallic SnSb has also been prepared by this route. The synthetic method is simple and does not require the use of very high temperatures, multi-step reactions or reaction under vacuum. Compounds were synthesised by the reduction of mixed metal oxides under 10% hydrogen in argon at moderate temperatures (approx. 450°C). The route affords some control over the stoichiometry of the product. High purity binary phases formed include CoSb 3 , CoSb, NiSb, Cu 2 Sb and SnSb. Owing to the significantly different reduction temperatures of the starting metal oxides, Mo 3 Sb 7 was formed with impurities of MoO 2 and Sb metal. CoSb 2 and NiSb 2 were formed with impurities of CoSb 3 and NiSb, respectively.