Solid solutions of β-K2Bi8-xSbxSe13 are an interesting series of materials for thermoelectric investigations due to their very low thermal conductivity and highly anisotropic electrical properties. In this work, we aimed to synthesize solid solutions of β-K2Bi8-xSbxSe13 type materials using powder techniques. The synthesis was based on mechanical alloying as well as sintering procedures. The products were studied in terms of structural features, composition and purity with powder x-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. Preliminary results on thermoelectric properties as well as IR reflectivity measurements are presented.