Cu-Ag particles with different molar ratio have been prepared in the hyperbranched polyester matrix by using ascorbic acid as a reducing agent. The third generation hyperbranched polyester has been synthesized by step by step polymerization using the first generation hyperbranched polyester as core molecular and 2, 2-dimethylol propionic acid as branched monomer. The synthesized hyperbranched polyester and Cu-Ag alloy were characterized by different analytical techniques such as FT-IR, 1H-NMR, UV-vis spectra, X-ray diffraction (XRD), SEM, Energy Dispersive X-ray (EDX), Laser particle size measurement, TEM, etc. The XRD and EDX studies confirm the formation of Cu-Ag alloy. The Laser particle size measurement, SEM and TEM studies show that the Cu-Ag alloy is well-dispersed particles with average size of 120 nm. The thermal properties of the Cu-Ag alloy have been studied by thermogravimetric Analysis (TGA). The results showed that the measurement values are close to the theoretical ones.