This paper presents the synthesis of Co-doped Al 2 O 3 catalysts, developed by our group, with porous structures and high surface areas. The catalytic activity of the materials obtained was evaluated in the catalytic decomposition of methane, which is an attractive method for CO/CO 2 -free production of hydrogen, particularly for fuel cell applications.The catalysts were shown to be active and stable in relation to the catalytic decomposition of methane reaction. It was observed that the catalytic performance is dependent on the catalyst characteristics and on the operational conditions employed.The conversion of methane increased with metal loading, reaction temperature and N 2 :CH 4 molar ratio.