In last years, the carbon nanotubes have been studied as an advanced metal catalyst support for proton exchange membrane fuel cell. This study focuses on the sonochemical treatment of multi walled carbon nanotubes (MWCNTs) as a platinum supporting material for proton exchange membrane fuel cell (PEMFC) by mixture of sulfuric acid and nitric acid and mixture of sulfuric acid and hydrogen peroxide. X-ray diffraction (XRD) and Infrared (IR) spectroscopy were used to characterize the surface of sonochemically treated MWCNT and nanostructured electrocatalyst Pt/MWCNT. According to the experimental results of this work, the surface of MWCNT can be more successfully functionalized with hydroxyl and carboxyl groups after sonochemical treatment by mixture of sulfuric acid and nitric acid. The particle size of prepared Pt -electrocatalyst on MWCNT was determined 3.4 nm by XRD.