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A novel strategy for the synthesis of CoSb₂ nanoparticles is demonstrated via preparation of novel organometallic complexes. Hydrated cobalt oleate (CoOl) and non-hydrated antimony oleate (SbOl) complexes are synthesized as precursors. The CoSb₂ nanoparticles are prepared by hot injection, which involves thermolysis of CoOl and SbOl in a non-coordinating solvent at 320 ℃. The coordination modes and distinct thermal behaviors of the intermediate non-hydrated SbOl complexes are comparatively investigated by thermo-analytical techniques. When the reaction temperature is increased, the particle size is found to increase linearly. The crystallinity of the CoSb2 nanoparticles prepared at 250℃ is amorphous phase without any peaks. CoSb₂ structural peaks start to appear at 300℃ and dominant peaks with high crystallinity are synthesized at 320℃. The potential chemical structures of non-hydrated SbOl and their reaction mechanisms by thermolysis are elucidated. The elemental composition and crystallographic structure of CoSb₂ nanoparticles suggest a bimodal interaction of the organic shell and the nanoparticle surface, with a chemical absorbed inner layer and physically absorbed outer layer of carboxylic acid.

Hot-Injection Thermolysis of Cobalt Antimony Nanoparticles with Co(II)-Oleate and Sb(III)-Oleate