The influence of the mechanical alloying processing parameters on the elaboration of AgCu-based bimetallic matrix composites reinforced by in-situ synthesized Cu2O has been studied. The milling time (20, 45 and 80 h) of the initial 72% mass Ag + 28% mass Cu micrometric powders mixture influences the particle size distribution of the obtained composite particles. After 80 h of mechanical alloying, AgCu/Cu2O nanoparticles of 60-80 nm are obtained and their chemical composition at bulk/surface level has been determined by X-ray diffraction and photoelectron spectroscopy. The effect of milling time on the thermal behavior of the powders samples has been studied by thermogravimetry and differential scanning calorimetry measurements in argon atmosphere. The argon chemosorbtive reaction from the particles surface has been identified and the binding energy (0.9-1.99 eV) has been calculated. The isothermal drop calorimetry and the linear thermal expansion measurements were used to evaluate the correlation between thermal stability and thermal expansion properties of the in-situ synthesized AgCu/Cu2O nanocomposite. (C) 2015 Published by Elsevier B.V.