Mechanical alloying is a powder processing technique used to process materials farther from equilibrium state. This technique is mainly used to process difficult-to-alloy materials in which the solid solubility is limited and to process materials where nonequilibrium phases cannot be produced at room temperature through conventional processing techniques. This work deals with the microstructural properties of the Al-20 at. % Cu alloy prepared by high-energy ball milling of elemental aluminum and copper powders. The ball milling of powders was carried out in a planetary mill in order to obtain a nanostructured Al-20 at. % Cu alloy. The obtained powders were characterized using scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The structural modifications at different stages of the ball milling are investigated with X-ray diffraction. Several microstructure parameters such as the crystallite sizes, microstrains and lattice parameters are determined