Nanocrystalline CoS 2 and NiS 2 have been successfully prepared through a solventothermal synthetic route at 130 o C. The final products are characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The sulfur-to-metal ratio of the as-prepared products is ca. 1.99-1 and 1.98-1 for CoS 2 and NiS 2 , respectively. TEM shows that with the change of solvents, the morphologies of the as-prepared sulfides can be controlled.