In the last years, photocatalytic materials has achieved an important role in several applications as water splitting, nitrogen fixation and degradation of organic pollutants for waste water decontamination. Among this class of materials, perovskite-based materials presents a great potential for catalysis under visible light. Bismuth Ferrite (BiFeO3) is a multiferroic magnetoelectric material with rhombohedral distorted perovskite structure (ABO3) showing ferroelectricity and antiferromagnetism at room temperature. Recently, BiFeO3 has been successfully applied as a catalyst for discoloration of some organic dyes in waste water due to their band gap (~2.3 eV) and controllable electron-hole separation owing the ferroelectric properties. However, the synthesis of BiFeO3 for the use as catalyst are focoused mainly in wet-chemical routes such as PVA and co-preciptation techniques. In this sense, BiFeO3 was synthesized by milling techniques and used as catalyst in the decontamination of Methylene Blue. The particles surface potential was measured by photo-assisted kelvin force microscopy (PKFM) in the dark and under visible light and the results were correlated with the morphology and the catalysis results.