The thermal decomposition of an alumina precursor, obtained by the emulsion evaporation technique, was investigated by thermogravimetry (TG) and differential thermal analysis (DTA). The thermal decomposition was completed in four steps between 100 degreesC and 550 degreesC. For each step, the activation energy was determined from the TG data by the Coats-Redfern procedure and the decomposition was discussed. The X-ray diffraction (XRD) data revealed that diaspore (beta -AlOOH) was formed during the emulsion evaporation. The resulting pure but porous alpha -Al2O3 powders were then calcined for 2 h at various temperatures between 600 degreesC and 1600 degreesC. The adsorption and desorption of N-2 on the calcined specimens at approximately 77 K was investigated. The variation of the total micro and mesopore volumes, the micropore volumes, the surface area and heat of adsorption as calculated from experimental data were discussed as a function of the calcination temperature. It was observed that the above mentioned properties reached a maximum at 800 degreesC, and then decreased rapidly by increasing temperature. It was concluded that it was possible to prepare fine alpha -Al2O3 powders whose specific surface areas varied between 20 and 90 m(2) g(-1) by changing the calcination temperature between 600 degreesC and 1600 degreesC.