The low-temperature solid-phase synthesis of high-purity CdTiO3 submicrocrystals has been achieved via two simple steps: firstly, CdO2 nanoparticles with the size of about 5 nm were precipitated from the reaction of 3CdSO(4) (.) 8H(2)O and H2O2 in an alkalescent aqueous solution (pH = 8.0) under the ambient condition; secondly, ilmenite-phase CdTiO3 powders with the sizes in the range of 150-350 nm could be produced by subjecting the as-prepared CdO2 nanoparticles and TiO2 powders to thermal treatment in air at 600 degrees C for 6 h. The as-obtained products were characterized by means of powder X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). (c) 2005 Elsevier B.V. All rights reserved.