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In this study, we present the preparation of a bulk material with a composition of 80GeTe2–20Ga2Te3 by combining mechanosynthesis and sintering. This composition cannot be prepared by conventional melt/quenching technique. The progressive evolution of the powder during ball-milling is followed by X-ray Diffraction (XRD) and Differential Scanning Calorimetry analysis. The final powder obtained is highly crystalline, but a glass transition temperature (Tg) is observed, indicating the presence of some amorphous phase remaining, allowing for its efficient sintering. By hot-pressing, a dense bulk material with a fine microstructure and a high electrical conductivity is obtained. The synthesis method described represents a simple and cost-effective way to produce tellurium-based materials of desired dimension with potential applications for optical storage or thermoelectric devices.