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Barium hexaaluminate, BaO·6Al<SUB>2</SUB>O<SUB>3</SUB>, exhibited excellent heat resistance in maintaining a large surface area. Preparation from hydrolysis of metal alkoxides was a superior process in deriving the large surface area of BaO·6Al<SUB>2</SUB>O<SUB>3</SUB>, to that from mixtures of BaCO<SUB>3</SUB>⁄γ-Al<SUB>2</SUB>O<SUB>3</SUB>. Direct formation of BaO·6Al<SUB>2</SUB>O<SUB>3</SUB> phase at low temperature plays the key role in retaining the fine particle size. The amount of water added for hydrolysis and the aging period of hydrolyzed precursors strongly influenced the surface area of alkoxide-derived BaO·6Al<SUB>2</SUB>O<SUB>3</SUB>. These effects of the preparation conditions originated from the difference in microstructure and chemical structure of the hydrolyzed precursors. Monodispersed fine precursor particles with high oxide content generated large surface area BaO·6Al<SUB>2</SUB>O<SUB>3</SUB>.
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