A solventothermal process has been developed to prepare CuFeSe 2 nanocrystallites at 230 o C with CuCl, FeCl 3 .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 CuFeSe 2 to be obtained. The final product was characterized by X-ray diffraction (XRD), Mossbauer spectroscopy and transmission electron microscopy (TEM).