Strong SERS effect for copper oxygenous compounds array synthesized from slightly acidic Cu(II) acetate solution using ac electrolysis is shown. The formation of cuprous oxide, Cu2O, with some metallic Cu-0 phase within pH range from 4.80 to 5.15 is demonstrated using X-ray spectroscopy (XRD), Fourier transform infrared (FTIR), and Raman spectroscopy. The presence of both CuO and acetate anions (CH3COO-) incorporated into the alumina during ac treatment were also detected in the thicker templates. It was found that a rod-shaped array of the aggregates in diameters from 80 to 120 nm exhibit relatively small electromagnetic enhancements of signals at 634 and 150 cm(-1), a common range for Cu2O when using for excitation a 1064 nm line laser. In contrast, intense surface-enhanced Raman bands of-carboxylate group, v(s)(COO), of acetate anion at 1366 and 1395 cm(-1) in 632.8 nm-excited spectrum were observed for the first time for these aggregates deposited into the alumina template with a diameter of about 15 nm. (C) 2003 Elsevier B.V. All rights reserved.