In order to synthesize the fine compound iron-doped nickel disulfide (NiS2) with environmentally friendly nickel, sulfur and iron powders, mechanical alloying (MA) was conducted for 8 hrs with SPEX Mill at a speed of 1000 rpm. In this process, stearic acid was added as a kind of process control agents (PCAs) to prevent the excessive cold welding. Meanwhile, for the purpose of getting nanocrystalline of Fe-doped NiS2 powder particles to improve the contact areas between the active materials, the wet milling process was also done for 30 hrs with normal hexane (C6H14) as a solvent PCA. The prepared powders were characterized by FE-SEM, XRD, EPMA, EDS and TEM. Finally, the charge/discharge properties of Li/Fe-doped NiS2 cells were investigated at room temperature by employing 1 M LiCF3SO3 (lithium trifluoromethanesulfonate) dissolved in TEGDME (tetraethylene glycol dimethylether) as the electrolyte. The initial discharge capacity of Li/Fe-doped NiS2 cell using wet milled powders as the cathode material is 792 mAh/g, which may indicate its high energy density and good future as cathode materials for lithium-ion batteries.