A simple and convenient polyol-mediated route has been developed to produce nanocrystalline Ag3SbS3 and Cu3SbS3 from AgNO3 and Cu(NO3)(2) and SbCl3 with thiourea at 197 degreesC. The products were characterized by Xray powder diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. Analysis shows that glycol agitated state and injection rate have a great effect on the purity of the final products. (C) 2002 Elsevier Science Ltd. All rights reserved.