A novel Al-Ce hybrid adsorbent with high sorption capacity for fluoride was prepared through the coprecipitation method in this study, and its preparation conditions were optimized. X-ray diffraction (XRD) and scanning electron microscope (SEM) results showed that the hybrid adsorbent was of amorphous structure and constituted by some aggregated nanoparticles. As the adsorbent had the zero point of potential at pH 9.6, it was very effective in fluoride removal from aqueous solution via electrostatic interaction. The results of sorption experiments including sorption kinetics, isotherms, and the effect of solution pH showed that the sorption of fluoride on the Al-Ce adsorbent was fast and pH-dependent. Especially, the adsorbent had high sorption capacity up to 27.5 mg g(-1) for fluoride at the equilibrium fluoride concentration of 1 mg L-1, much higher than that of the conventional adsorbents. Fourier transform infrared (FTIR) analysis and zeta potential measurement showed that the hydroxyl groups and the protonated hydroxyl groups on the adsorbent surface were involved in the fluoride adsorption. (C) 2010 Elsevier B.V. All rights reserved.