Polyacrylonitrile (PAN) layers were cast from dimethyl-formamide solutions onto quartz substrates by spin coating and subsequently annealed at up to 1000 degrees C in N(2) atmosphere. Carbonization was catalyzed by nickel or cobalt added to the solution as acetate salts. The synthesized films were approx. 970 nm thick and were characterized by Raman and infrared spectroscopy as well as thermogravimetric and electrical conductance measurements. We discuss the effects of carbonization temperature and metal concentration on the morphology, composition and electrical properties of the formed carbon layer. Increasing the amount of catalyst and the pyrolysis temperature was beneficial for the process and resulted in carbonaceous films with a higher degree of structural order as evidenced by the decreasing Raman I(D)/I(G) ratio and the increasing electrical conductivity of the films. Cobalt is a better catalyst for PAN carbonization than nickel as far as the structure of the product film is concerned. (C) 2011 Elsevier B.V. All rights reserved.