In this Letter, sodium dodecyl sulfate (SDS) was applied not only as surfactant, but also as sulfur source to produce AgInS 2 . Nanostructures were characterized extensively by means of X-ray diffraction, energy-dispersive X-ray analysis, scanning electron microscopy, transmission electron microscopy and infrared spectrum. Nanoparticles have been successfully synthesized through an microwave-ultrasonic method by employing mixture of InCl 3 , AgNO 3 as silver precursor and SDS in 40 ml of propylene glycol as a solvent. This method is novel, simple and can be easily controlled. Effects of different parameters such as power, and time of irradiation were investigated.