The possibility of the ac formation of a novel nanostructured material within the alumina pores composed mainly of Cu-0/Cu1.76S has been shown. For this purpose an aqueous acidic solution composed of copper sulphate, magnesium or aluminium sulphate and thiourea was used. The formation of copper sulphide was confirmed by the sharp peaks at about 1100 and 249 cm(-1) in the compensated FTIR and Raman spectra, respectively. In addition, X-ray diffraction patterns taken from the synthesized product within the alumina pores indicated only a broad shoulder at 20 between 42degrees and 47degrees, which could be attributed to the diffraction of microcrystalline Cu-0 and most likely to microcrystal line non-stoichiometric copper sulphide, Cu1.76S, known as digenite. These species colour alumina templates grown in the sulphuric acid bath in unusual for Cu-0 arrays tints from grey to deep black. (C) 2004 Elsevier B.V. All rights reserved.