This paper presents a novel technique to create Al2O3 hollow spherical nanoparticles. It used Al(OH)(3) which was synthesized with Al-2(SO4)(3) and NaOH, and the C-Al(OH)(3) core-shell nanoparticle as intermediate phases. The Al2O3 hollow spheres were achieved by the calcination of the carbon cores and the dehydration of Al(OH)(3). The chemical composition, morphology, size and superficial crystal structure of the nanoparticles were characterized with TEM, XRD, TGA, FTIR and BET. The result shows that the average diameter of the C-Al(OH)(3) core-shell nanoparticles is about 25 nm, the thickness of the Al2O3 shell is about 5 nm and the surface area is 215.2 m(2)/g. The procedure for the formation of Al2O3 hollow nanoparticles is discussed in details. (C) 2008 Elsevier B.V. All rights reserved.