Hexagonal close-packed Ni nanoparticles were synthesized using a heat-treating technique with the precursors prepared by the sol-gel method.The synthesis condition,structure,and morphology of the samples were characterized and analysed by thermogravimetric analysis (TG),differential thermal analysis (DTA),X-ray diffraction (XRD) and transmission electron microscopy (TEM).Results indicate that the hexagonal close packed Ni nanoparticles were synthesized at a heat-treating temperature of 300℃.The cell constants are calculated at a=0.2652 nm and c=0.4334 nm.The average grain size of the hexagonal close-packed Ni particles evaluated by Scherrer equation is about 12 nm.The phase transformation from a hexagonal close-packed Ni to a face-centered cubic Ni structure occurred when the heat-treating temperature was increased.