A series of samples, noted AlxCe1−x has been prepared by hydrolysis, from γ-Al2O3 and CeO2. These samples were calcined under air at 450, 900 and 1200 • C, and then characterized by specific surface area, X-ray diffraction and thermoreduction programmed under H2. Obtained results show that after calcination at 450 and 900 • C, the cerium decreases the surface of alumina. Results of X-ray diffraction and thermoreduction programmed under H2 experiments showed that the samples are constituted of: γ-Al2O3 and CeO2. The global consumption of hydrogen increase with rate of CeO2 added. At 1200 • C, the sintering of the samples is very important and γ-Al2O3 is transformed into the α-phase. The decrease in specific surface area is more accentuated for Al1Ce0 sample, since sintering occurs due to the growth in crystallite size. Thermoreduction programmed under H2 experiments show that reduction of CeO2 much more accentuated for ceria samples or its decrease can reflect some alterations of the nature of interactions between Al2O3 and CeO2.