The purpose of this paper is to investigate the possibility of rod-like Al2TiO5 formation via a mechanical activation process. A QM-ISP-4 Planetary Mill was employed to activate mechanically the mixtures of anatase and corundum in air at room temperature for different times. The milled powder mixtures were then sintered in air at 1300°C for 1 h. The XRD results showed that the milled powder mixtures were completely transformed into Al2TiO5 after sintering, except the mixtures milled for 5 and 10 hours. The SEM observations showed the typical morphology of rod-like Al2TiO5 vary in the range: widths from 0.6 to 1.2 μm, and lengths from 3.0 to 6.0 μm. The rod-like Al2TiO5 formation was attributed to the positive effects caused by the mechanical activation.