The semi-magnetic semiconductor thermoelectric alloy Pb 1−x Yb x Te (0.0>x<0.075) was synthesized by solid-state microwave. Polycrystalline was prepared by high-purity powders for the three elements Pb, Yb, and Te from microwave irradiation-induced equilibrium reaction of initial components to obtain ingots with a large grain size. The morphology of the microstructure and polycrystalline stoichiometric ratio for these ingots was performed using scanning electron microscopy (SEM) and energy dispersive X-ray spectra (EDX). High-quality polycrystalline thin films of Pb 1−x Yb x Te were deposited onto clean glass substrates using the vacuum evaporation technique at 10 −6 mbar. The structures of the polycrystalline powders and thin films were examined by X-ray diffraction (XRD) patterns. A rock salt structure was observed, and the lattice constant increased with increasing amount of Yb, but not in accordance with Vegard's law. The thermoelectric properties were measured at a temperature range of 298–523K. Carrier concentrations of the films were determined using Hall effect measurements at 300K.