Nickel powders were prepared from an aqueous nickel acetate solution and hydrazine hydrate using diethanolamine as the nonaqueous organic solvent in the conventional and microwave synthetic method. It was investigated that microwave non-thermal effect and synthetic condition affect the preparation of nickel powders by means of X-ray diffractometry, scanning electron microscopy, thermal gravymetry analysis, and X-ray photoelectron spectroscopy analysis. Compared with the conventional synthetic method, less of aggregation, smaller particle size, and more uniform distribution of particle size were obtained in the microwave synthetic method due to the non-thermal effect of microwaves.