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Since prepared substrates offer an appropriate method for the selective production of uniform arrays of aligned CNTs and CNFs, it is important to illustrate the influence of different catalysts on the resulting nanostructures. This investigation characterizes the activity of three catalysts — iron in alloyed form as stainless steel, nickel, and platinum — on carbon nanostructure formation under identical conditions in an ethylene/air nonpremixed flame. We have synthesized well-aligned multi-walled CNTs (on Ni) and CNFs (on stainless steel). The third transition metal Pt produces CNF structures of a different kind and its activity has not been previously characterized in flames. The catalyst and gas-phase conditions leading to the formation of these different structures are discussed.