This paper reports on the synthesis of CuInS2 nanostructure via an ultrasonic assisted method by employing different sulfur source. Morphology, structure and composition of the obtained products were characterized by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), scanning electron microscope (SEM), infrared (IR) spectrum, and photoluminescence (PL) spectroscopy. The effects of ultrasonic irradiation, power and time of irradiation, surfactant, and type of copper source were investigated. (C) 2012 Elsevier Ltd. All rights reserved.