A set of LaMnO3 and LaCoO3 catalysts was prepared through different synthesis procedures. The selected techniques included the sol-gel method, flame hydrolysis from aqueous solution, complexation through EDTA and solid-state reaction. The last was accomplished through reactive grinding by ball-milling either in a vibration mill or in a planetary mill. EDTA complexation was applied for LaCoO3 only and did not improve significantly catalyst activity or stability, with respect to other techniques. Ball-milling never allowed obtaining a pure perovskitic phase, at least under the most energetic grinding conditions permitted by our apparatus. The highest activity for the catalytic flameless combustion of methane was obtained with the sol-gel prepared samples, though thermal resistance revealed insufficient for high temperature applications. A bit lower activity, but coupled with good thermal stability was obtained with the samples prepared through flame hydrolysis. (C) 2004 Elsevier B.V. All rights reserved.