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乙醇为溶剂超临界干燥法制备纳米Al_2O_3 被引量:4

Use of anhydrous ethanol as solvent to prepare nano A1_2O_3 by a supercritical drying method
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摘要 以硝酸铝为原料,柠檬酸为分散剂,无水乙醇为溶剂,采用溶胶-凝胶结合超临界干燥的方法制备了纳米AlOOH。经过500~900℃焙烧后得到纳米-γAl2O3。考察了溶液pH值、硝酸铝与柠檬酸物质的量比对AlOOH粉体,以及焙烧温度对-γAl2O3两者形貌和尺寸的影响。采用TEM、XRD、IR对超细粒子的粒径、形貌进行了表征。结果表明,制备溶胶时的pH值和柠檬酸的加入对经超临界干燥所得的AlOOH的形貌和尺寸有明显影响。在pH=3,n(C6H8O7)∶n(Al(NO3)3)=1∶2的条件下可得到纤维状纳米AlOOH(直径为1~10 nm,长为30~40 nm)。该AlOOH经500~900℃焙烧后可得纤维状纳米-γAl2O3,其直径为1~10 nm,长为30~70 nm。 Nanosized AIOOH has been prepared by a combination of sol-gel and supercritical drying methods, using aluminum nitrate as the raw material, citric acid as dispersant and anhydrous ethanol as solvent. Nano γ- Al2O3 was obtained after calcination of the A1OOH at 500 - 900 ℃. The effects of varying the pH of the synthe- sis solution and the ratio of aluminium nitrate to citric acid on the particle size of AlOOH as well as the effect of varying the calcination temperature on the particle size of γ-Al2O3 were investigated. The morphology, particle size and structure of the products were characterized by TEM, IR and XRD. It was found that both the pH of the solution during the preparation of the sol-gel and addition of citric acid significantly affected the morphology and size of the AlOOH particles. At pH = 3 with n (citric acid) : n (aluminum nitrate) = 1 : 2, fibrous nano AlOOH particles (with a diameter of 1 - 10nm and a length of 30 - 40nm) were obtained. Calcination of the re- suiting nano AlOOH at 500 - 900 ℃. afforded fibrous nano γ-Al2O3 particles with a diameter of 1- 10 nm and a length of 30 - 70 nm.
出处 《北京化工大学学报(自然科学版)》 EI CAS CSCD 北大核心 2008年第5期8-12,共5页 Journal of Beijing University of Chemical Technology(Natural Science Edition)
关键词 氧化铝 柠檬酸 溶胶-凝胶 超临界干燥 alumina citric acid sol-gel supercritical drying
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