The mechanically activated annealing process were used to produce Cu3Si compound. This process results from the combinaison of two steps, the first is a mechanical activation of the 3Cu + Si powders mixture, the second consists of the annealing of as-milled powders. Based on X-ray diffraction experiment, scanning electron microscopy, the as-milled powders and M2AP end-products were characterized. Various process controlling parameters such as mechanical activation conditions were studied. In the same time, a sutdy of the reactivity ofCu(3)Si towards CuCl were performed to compare the M2AP end-products behavior with that of the Cu3Si reference powder.