A simple, low-temperature, catalyst-free solution-based approach was developed to obtain heterostructures of group VI semiconductors. The formation of bone-like crystalline nanorods of SexTe1-x/Te/SexTe1-x heterojunctions with lengths up to 1.5 mum were achieved by controlling pH and temperature of aqueous reaction media, without the participation of catalyst. Samples as-prepared were characterized by using X-ray diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HREM). Energy-dispersive X-ray (EDX) analysis was also performed to identify the composition distribution of a single heterojunction. It is reasonable to expect that the incorporation of trigonal Te nanorods with phase-separated trigonal SexTe1-x alloys may intrigue investigating in the possible changes in its energy band structure and interface states physics together with consequent new electricity, thermoelectric, and transport behaviors. (C) 2003 Elsevier B.V. All rights reserved.