Synthesis of Nanocrystalline α-Al2O3 Using a 2-Step Calcination Method
Nanocrystalline α-Al2O3 powders have been prepared by the pyrolysis of a resin compound of aluminum with polyester by a two-step calcination process. A polymeric precursor was prepared using a complexing agent to keep the metal ions in homogeneous solution, which gives sufficient flexibility for the system to exist homogeneously throughout the reaction without undergoing precipitation. The metal-ion-polyester resin forms the precursor material on complete polymerization reaction of aluminum nitrate, citric acid and ethylene glycol. A single-phase α-Al2O3 powder resulted after calcinations above 1150°C, but during heat treatment α-Al2O3 particles grow very fast by coalescence. So 2-step calcination was used, where the first step was done in a reducing atmosphere at above 1150°C and second calcinations were done in oxidizing atmosphere at the relatively low temperature of 1000°C. The precursors and the heat-treated final powders have been characterized by X-ray diffractometry, thermogravimetry , transmission electron microscopy(TEM), and BET surface area analysis. The nanocrystalline α-Al2O3 particles obtained by this 2-step calcinations method had an average specific surface area of >170m2/g, with an average particle size between 40 and 60nm.
T. Ohji, T. Sekino and K. Niihara
M.J. Cho et al., "Synthesis of Nanocrystalline α-Al2O3 Using a 2-Step Calcination Method", Key Engineering Materials, Vols. 317-318, pp. 199-202, 2006