Ilmenite is one of the most common minerals on earth crust, often found in igneous rocks and black sands of alluvial deposits and can be located in different parts around the world; it is used as natural source of TiO2 and Fe and as catalyst in photodegradation processes [1].Research performed at Grupo de Investigación en Química Estructural -GIQUE and Grupo de Investigaciones en Minerales, Biohidrometalurgía y Ambiente -GIMBA using ilmenite-rich black of Barbacoas (Nariño, Colombia) for photocatalytic applications found that the specific surface area of the mineral (2.4-4.2 m 2 /g) is quite low compared to that of common photocatalysts (20-50 m 2 /g) [2,3].With the aim for inducing morphological changes that lead to an increase of the surface area, that would imply more active sites available for reaction; this research proposes to submit ilmenite-rich concentrates to high energy ball milling assisted by acid solutions of acetic acid and sulfuric acid, since acids can cause changes in the distribution and oxidation state of elements on the mineral surface, thus producing pores and cracks on the surface [4,5].However, high-energy milling in the presence of acid solutions can significantly modify the crystallography of nanostructured materials, therefore, it is important to evaluate the effect of the stress applied on particle size, surface area and composition, while tracing changes in the microstructure of ilmenite.The product of the acid treatment was obtained by evaluating the concentration of acid in the solution 1, 3 and 5 w/v %, time (1-3 h), milling speed 650 rpm, ball to power weight ratio BPR (3:1, 10:1 and 20:1) and size of grinding medium (4.0 and 4.8 mm).