Mesoporous materials are both scientifically and technologically important because of the presence of voids of controllable dimensions at atomic, molecular, and nanometric scales. Over the last decade, there has been both an increasing interest and research effort in the synthesis and characterization of these types of materials. Well ordered mesoporous alumina materials with high surface area and a narrow pore size distribution were synthesized using the anodization process. The purposes of this work are to study the physical and chemical changes in the properties of mesoporous alumina films produced by anodization in sulphuric acid by different pretreatments on the aluminum surface such as Mechanical Polishing [MP] and Electropolishing [EP]. The morphologic and physical characterizations of the alumina film samples were carried out by Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD). The average mesoporous diameter was 17 nm, and the morphological shape was equiaxial; thus, that pore distribution was the smallest of all with the homogeneous distribution.