A convenient hydrothermal decomposition process has been developed to prepare cupric oxide shuttle-like nanocrystals using CuCl2.H2O and NaOH as the starting materials. The product was characterized by X-ray diffraction, scanning electron microscopy, Raman spectra and X-ray photoelectron spectroscopy. The results showed that the as-prepared CuO shuttle-like crystals have regular shape, uniform size distribution and with high yield. (C) 2003 Elsevier Science B.V. All rights reserved.