CdIn2Se4 and Cu0.5Ag1.5InSe3 are high-performance thermoelectric materials. In this study, both CdIn2Se4 and Cu0.5Ag1.5InSe3 powders were synthesized using a microwave and solution method followed by annealing in nitrogen atmosphere. CdIn2Se4 was synthesized by two routes. First, CdSe was prepared using a microwave method. Second, In metal was prepared using a solution method. The prepared metals were annealed in nitrogen atmosphere. From the x-ray diffraction (XRD) results, CdIn2Se4 was observed as the main phase with CdSe and In2O3 as contaminant phases. The synthesis of Cu0.5Ag1.5InSe3 was also divided into two steps. First, CuAg and Se were prepared using a microwave method. Second, In metal was prepared using a solution method. The prepared metals were annealed in nitrogen atmosphere. From the XRD results, Cu0.5Ag1.5InSe3 was observed as the main phase with Cu0.5-xAg1.5-yInx+ySe and Se as contaminant phases. © 2014 TMS.