Bimetallic platinum-vanadium nanoparticles have been successfully synthesised by high temperature thermal decomposition of metal precursor salts. Vanadium is a highly reactive metal and poses considerable difficulty in synthesising metallic nanoparticles, while platinum has low reactivity where nanoparticles are easily synthesised. The difficulties associated with the reduction of vanadium salt were circumvented by the use of high boiling point solvents and selected surfactants. Co-reduction using platinum precursors compatible with the high temperature processes was required for bimetallic nanoparticle synthesis. The chemical synthesis route described is novel, robust and highly reproducible. Microstructural characterisation of nanoparticles synthesised as described, using transmission electron microscopy, reveals single-crystal particles.