A solventothermal process has been developed to prepare CuFeSe2 nanocrystallites at 230 degrees C with CuCl, FeCl3 . 6H(2)O and Se powders as starting materials. The effect of solvent on the product has been studied and in our experiments, pyridine is the only solvent that can lead CuFeSe2 to be obtained. The final product was characterized by X-ray diffraction (XRD), Mossbauer spectroscopy and transmission electron microscopy (TEM).