The multi-walled carbon nanotubes (MWNTs) were treated by different methods with mixed acid to introduce defects. Then the Pt/MWNTs catalyst was synthesized by polyol method. After that, a two layer buckypaper was prepared using a filtration method. The electrochemical characteristics were studied by cyclic voltammetry (CV) and liner sweep voltammetry (LSV) techniques. The results showed that the ultrasonic treatment is the best way to treat the MWNTs and increases the Pt loading in the catalyst compared with other treatments. The CV performance of the Pt/MWNTs-Ultrasonic catalyst is equivalent with the Pt/C JM catalyst and the LSV result of Pt/MWNTs-Ultrasonic catalyst is better than the Pt/C JM catalyst. The Pt/Buckypaper catalyst layer also showed good ORR performance. With the advantage of easy preparation, the Pt/Buckypaper catalyst layer has a potential to be widely used in PEMFCs.