Ceramic microspheres have been used in various applications, related to the nuclear, pharmaceutical, chemical, medical, environmental, biotechnology, etc. It is possible to obtain, by internal gelation method, microspheres of different ceramic materials, dense or porous (with controlled porosity) and different sizes. However, the major obstacle is the formation of cracks on drying and / or calcination, which can hinder their use. This study have an objective at the production of alumina (Al 2 O 3) based microspheres by internal gelation process, varying processing parameters in order to control the chemical and physical characteristics such as size, porosity, specific surface area, etc., in addition to specific characteristics that enable their application in filling of the elution columns of 99 Mo-99m Tc generators. It was developed a simple and efficient method of washing treatment of the microspheres, which enables the extraction of a significant portion of the organic phase present prior to drying and calcination; thus virtually eliminates all cracks that arise during drying, and particularly in calcination step. In addition, process parameters were varied for controlling the porosity and specific surface of the microspheres. Were also characterized in parallel, two transition aluminas in the form of powders currently used in filling of elution columns of 99 Mo-99m Tc generator so as to get an idea of the current requirements for physical properties of the filling material.