The present work concerns the intermetallic compound (IMC) existing in the Ag-Sn system and its potential use in electronics as attachment materials allowing the adhesion of the chip to the substrate forming the power module. First, we present the synthesis protocol in polyol medium of a compound with the chemical formula Ag 5 Sn 0.9 belonging to the solid solution of composition located between 9 and 16 at.% Sn, known as solid solution ζ (or ζ-Ag 4 Sn). This phase corresponds to the peritectic invariant point at 724 • C. Differential thermal analysis and X-ray dispersive analysis confirm the single-phased (monocrystalline) nature of the Ag 5 Sn 0.9 powder issued after synthesis. Scanning electron microscopy shows that Ag 5 Sn 0.9 particles are spherical, and range in submicronic size of around 0.18 µm. X-ray diffraction analysis reveals that the ζ phase mostly exists under the two allotropic varieties (orthorhombic symmetry and hexagonal symmetry) with however a slight excess of the hexagonal variety (60% for the hexagonal variety and 40% for the orthorhombic variety). The lattice parameters resulting from this study for the two allotropic varieties are in good agreement with the Hume-Rothery rules.