Bismuth–antimony alloy nanoparticles have been synthesized by a facile solvothermal method using N,N-dimethylformamide and ethylene glycol as solvent/reducing agent; BiCl 3 , SbCl 3 and Bi(NO 3 ) 3 as precursors; and citric acid as a surface modifier/stabilizing agent. The particle size and size distribution of Bi nanoparticles were analyzed as a function of the synthesis conditions: molar ratio of precursor to surfactant, precursor concentration and reducing agent. Synthesis of Sb and Bi 0.88 Sb 0.12 under similar conditions was also investigated. The phase purity of nanoparticles was confirmed from X-ray diffraction and thermogravimetry and the nanoparticle morphology was investigated by transmission electron microscopy. A case study of Bi nanoparticles with detailed analysis of the particle morphology and size distribution of the nanoparticles is reported.