Nanocrystals of CdO have been obtained by the decomposition of the cupferron complex in the presence of tri-n-octylphosphine oxide (TOPO) under solvothermal conditions. The precursor:TOPO ratio plays an important role in determining the size of the nanocrystals. The nanocrystals have been characterized by electron microscopy, absorption spectroscopy and fluorescence spectroscopy, besides X-ray diffraction. The CdO nanocrystals are single crystalline and show evidence for quantum confinement. CuO nanocrystals could also be prepared by the decomposition of the cupferronate under solvothermal conditions, the particle size being controlled by the initial precursor concentration. (C) 2004 Elsevier B.V. All rights reserved.