Abstract: Nickel boride catalyst is prepared by the reaction of KBH₄ with Ni(Ⅱ) salt. Nickel boride samples prepared by different methods of after-treatment were characterized by chemical analysis, differential thermal analysis, X-ray diffraction and electrochemical tests. Experimental results indicated that catalyst samples of widely different boron content were oxidized almost at the same potential. However, in order to get more active catalyst for waterproofed electrode, the atomic ratio Ni/B of catalyst should be carefully controlled. It does not mean that the Ni/B ratio of the catalyst should be controlled at certain fixed value. We would only like to emphasize that, in order to get better results, the method of catalyst processing should be in accordance with the method of electrode fabrication. In other words, the optimal Ni/B ratio depends on the method of electrode fabrication. Some fuel cell anodes with nickel boride catalyst have been already running contineously at 50ma/cm² for more than 3000 hours without serious deterioration.