Thermo catalytic decomposition of methane using Ni-Al and Ni-Cu-Al catalyst prepared by fusion of the corresponding nitrates is studied. The effects of catalyst calcination temperature on the hydrogen yields and the characteristics of the carbon obtained are studied. The role of copper has been also analyzed. Whatever the calcination temperature, all the catalysts show a high and almost constant hydrogen yield without catalyst deactivation after 8 h on stream, which confirms the good performance of this kind of catalysts. The presence of copper enhances the hydrogen production and the best results were obtained using catalysts calcined at 600 degrees C. Cu has a strong influence on the dispersion of Ni in the catalysts and inhibits NiO from the formation of nickel aluminate even at high calcinations temperatures, which facilitates the formation of the metallic Ni active phase during the subsequent catalyst reduction step. All catalysts tested promote the formation of very long filaments of carbon a few tens of nanometers in diameter and some micrometers long. The structural properties of these carbon filaments highly depend on the presence of Cu:Ni-CuAl catalysts promote the formation of a well-ordered graphitic carbon while Ni-Al catalysts enhance the formation of a rather turbostratic carbon. (c) 2007 Elsevier B.V. All rights reserved.