Solvothermal Coordination-Reduction Route to gamma-NiSb Nanocrystals at Low Temperature

A very mild synthesis of nanocrystalline gamma-NiSb via a novel solvothermal coordinationreduction process is reported here. The reaction of the mixture of NiCl2, antimony, and KBH4 was carried out in ethylenediamine (en) at 140°C for 24 h. X-ray powder diffraction and transmission electron microscope images show that the products are hexagonal gammaNiSb phase and well crystallized with an average size of about 15 nm. The reaction proceeds through a metallic nickel intermediate. The morphology of the products was influenced markedly by the solvents, and a dendritic crystal of NiSb was obtained in diethylamine. The products were also investigated by UV/vis absorption, photoluminescence, X-ray photoelectron spectra, and Fourier-transform IR.