Abstract: Metallic nickel powders was synthesized in stainless steel autoclave at different temperature,using absolute ethanol as solvent and reductant.The product was characterized by X-ray powder diffraction（XRD）,scanning electron microscopy（SEM） and transmission electron microscopy（TEM）.XRD results show that the as-prepared sample have different crystal structures at different reaction temperatures.It is face-centered cubic（fcc） nickel under 230℃,and above 300 ℃.However,there are both fcc and close-packed（hcp） Ni coexisting in the as-prepared sample between 250℃ and 280℃.The SEM and TEM images indicate that the as-prepared samples synthesized at 400℃ is polyhedron with relatively regular structure and smooth surfaces,which have the diameter ranging from 1 to 2μm.There is nickel microspheres with not regular structure when the reaction temperature is 250℃.Mixtures of microspheres,polyhedron and microspheres with some apertures are discovered in the as-samples when the temperature is 300℃.The magnetic properties of the as-sample nickel was investigated.The mixture of fcc and hcp has relatively low saturation magnetization and remanent magnetization,but the coercivity is high.