Nanoparticles of the CuInTe2 (CIT) and CuInSe2 (CIS) alloys have been prepared using the microwave-assisted polyol method. In this simple and quick reaction the polyol is both the solvent and the reducing agent. XRD studies show that nanoparticles of CIT and CIS are formed in the body-centered tetragonal structure and their average diameters are similar to94 and similar to83 nm, respectively. Electron microscopy studies show that these formed particles are poorly aggregated with a mean diameter of 100 and 85 nm, respectively. The products have been characterized by different analytical techniques, and the electronic properties have been measured using photoacoustic spectroscopy (PAS).