Reactions of GaCl3 and Sb(SiMe3)(3) in a 1:1 molar ratio in different solvents (pentane, hexane, toluene, and xylene) are described. The resulting GaSb was characterized by electron and X-ray diffraction studies, energy-dispersive X-ray (EDS) analysis, and transmission electron micrography (TEM) studies. The particle size and chemical composition was controlled by the solvent. The size of the GaSb nanoparticles varied between 10 and 50 nm. (C) 2000 Elsevier Science Ltd.