Thermoelectricity is a green method of energy production by converting waste heat into electricity. Silicides and selenides are candidate materials for thermoelectric applications due to their high performance in their operating temperature range. Additionally, they are composedof abundant and negligibly toxic elements. The current study focuses on the fabrication of alternative thermoelectric materials, aiming todevelop compounds with advanced thermoelectric properties. Pure Mg2Si andAl-doped Mg2Si samples are synthesized by Pack Cementation (PC), and Ag2Se powder is produced via Ball Milling (BM). The chosen synthesis methods are suggested as environmentally friendly, fast and economic. The samples were structurally characterized by X-ray diffraction (XRD), while the morphology and the chemical composition were studied by X-ray photoelectron spectroscopy (XPS)and scanning electron microscopy (SEM). In the case of magnesium silicide, the thermoelectric phase was formed without residual traces of the initial elemental powders. The Al addition diffused in the material homogeneously and no secondary phases were developed. Regarding the Ag2Se powder, α-phase (low temperature) was obtained after 2.5 h of mechanical alloying (BM) the elements.SEM and XPS analysis detected traces of unreacted Ag and Se, indicating that the ball milling process should last longer to achieve a complete reaction between the elements.