The novel polygonal flake like Ag8SnS6 crystal, Cu2FeSnS4 flaky, and well-dispersed Cu2CoSnS4 nanoparticles were successfully prepared via a convenient hydrothermal reaction route at relatively low temperature, which was avoiding the use of high temperature treatments or toxic organic solvents. The products were characterized by means of X-ray powder diffraction (XRD), transmission electronic microscopy (TEM), X-ray photoelectronic spectra (XPS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). It was found that the reaction temperature played a key role for the formation of the target products. (C) 2003 Elsevier Science Ltd. All rights reserved.