A low temperature surfactant-assisted hydrothermal. synthesis route has been successfully developed for the preparation of high quality chalcostibite (CuSbS2) nanorods. The surfactant concentration is a key factor influencing the quality (size, shape) of the final products. A possible mechanism is proposed for the formation of chalcostibite nanorods. Several techniques including XRD, SEM, TEM and XPS were used to characterize the as-prepared chalcostibite nanorods. (C) 2003 Elsevier B.V. All rights reserved.