The present work aims to produce TixCu100-x (x = 90, 80, 70, and 60) amorphous alloys by using high energy ball mill. The microstructure and possible formation of amorphous phases were characterized employing laser granulometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The amorphous-crystalline transformation at high temperatures was studied according to differential scanning calorimetry (DSC) and XRD. The Ti80Cu20 alloys were obtained in an amorphous state after 30 h of mechanical alloying, and the amorphous phase is stable up to 340 °C. At higher temperatures, this alloy crystallizes, forming the intermetallic compound Ti2Cu, and a substitutional solid solution Ti(Cu).