Pure CdTe and CuInSe2 are prepared with high yields and short reaction times starting from metal or binary alloy powders and irradiating the mixture with a microwave radiation of a 2.45 GHz of frequency and 1000 W of power under argon atmosphere. It was possible to successfully synthesize extremely pure CuInSe2 single crystalline phase, differently from a multi-phase mixture as expected from the phase diagram Cu2Se-In2Se3. XRD and SEM analyses, performed for the characterization, have confirmed the success of the process