Technetium-99m is the clinically most used radionuclide worldwide. Although many techniques can be applied to separate 99Mo and 99mTc, the most commonly used method is the column chromatography with alumina as stationary phase. However, the alumina nowadays used has limited adsorption capacity of molybdate ions which implies the need to develop or improve materials to produce high specific activity generators. In this paper, alumina was obtained by a solid state method and heat treatments at different conditions. The powders had a microstructure with porous particles of ??, ??, ?? and ??-Al2O3 phases as well as specific surface area between 36 and 312 m2 g-1. Most interesting results were reached by powders calcined at 900oC for 5 hours which had high chemical stability and a molybdenum adsorption capacity of 92.45 mg Mo per g alumina.