The decomposition of methane into hydrogen and carbon was studied on Fe-Cu catalysts of Raney-type. The activity of the catalysts was assessed by comparing the experimental conversions with the calculated equilibrium conversions for each set of experimental conditions. The stability of the catalysts was assessed by comparing the maximum conversions with the conversions at the end of 5-hour tests. The carbon deposits obtained consist mostly of carbon nanofibers. Good results were obtained when the Fe-Cu Raney-type systems were thermally treated in situ at 600 degrees C, as a result of incipient alloy formation. These catalysts showed higher stability than the monometallic Raney-Fe catalysts. (C) 2009 Elsevier B.V. All rights reserved.