The Ca5Bi3 intermetallic compound was synthesized by milling Ca and Bi. Ca5Bi3 was obtained using a high-energy mill. A stoichiometric mixture of elemental powders was formed after three hours of milling. Next, the grade reagents, calcium and bismuth, were melted by heating at 1613 K for 12 h in sealed steel ampoules to prevent oxidation. The intermetallic compound was compacted using a hot isostatic press with 300 MPa and sintered at 673 K. The compound was characterized by chemical analysis, X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The product contains 1.68% Ca, 94.56% Bi and 5.43% O after milling, melting and press-sintering.