This work describes the use of focused, high-intensity light from a Ti: sapphire laser that generates femtosecond pulses to irradiate mixture of CeO2 and Tb4O7 under ambient conditions. The prepared samples were investigated by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM). XRD and XPS measurement results demonstrated that solid solution CeTbO3+delta with cubic fluorite structure has been synthesized on the irradiated target surface. SEM micrographs showed that the ultra-short laser irradiation resulted in the formation of foamy structure and spherical particles with size varying from about 30 to 200 nm. The formation mechanism has been discussed in detail. (c) 2006 Elsevier B.V. All rights reserved.