NiS was synthesized were prepared by hydrothermal and mechanical alloying routes, respectively, and their microstructures as well as physical and electrochemical properties have been characterized and compared. Based on XRD and SEM analyses, the NiS crystallites with nanoplate structure formed directly during a hydrothermal process. Compared with the mechanical alloying route, the hydrothermal route led to better dispersed nanoparticles with a narrower size distribution. And the electrochemical properties of the materials were characterized by charge-discharge testing and Cyclic-voltammetry. NiS were prepared by hydrothermal show proper cycling properties, its first discharge specific capacity was 584.6mAh/g.