We report the synthesis of bulk prismatic single crystals Of M2S3 (M = Sb, Bi) via a novel hydrothermal process, using SbCl3 or BiCl3 and sulfur as the raw materials at 180degreesC for over 7 days in the presence of diethylammonium chloride (DEACl) or tetraethylammonium chloride (TEACl), and Sb2S3 nanorods through a similar process in the presence of hydrazine hydrate. The products were characterized by various techniques, including X-ray powder diffraction (XRD), X-ray single crystal diffraction and field emission scanning electronic microscope (FESEM). The possible growth mechanism of single crystals was also discussed. (C) 2004 Elsevier B.V. All rights reserved.