Thermogravimetric (TG) curve of the dark brown precursor which was prepared by the emulsion evaporation technique, was obtained under the nitrogen atmosphere. The thermal decomposition of the precursor which was completed in four steps, was investigated by the Coats- Redfern procedure by using the TG data. Fine alumina powder was obtained from the precursor which was calcined at 1000 °C for two hours, after burning its organic fractions. The particle size distribution (PSD) of the powder was determined and its photographs were taken by an electron microscope. It was determined that the particles, whose sizes were between 0.8-30.0 pm, were composed of inagglomerated spheres, the insides of which wee porous.