Preparation of Ta2O5 aerogels catalyzed by different kinds of acids
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摘要: 采用溶胶-凝胶技术,以乙醇钽为前躯体,乙醇为溶剂,分别以盐酸、硝酸、硫酸为催化剂,结合CO2超临界干燥技术制备了Ta2O5气凝胶。研究发现:硫酸作催化剂的体系,其胶凝时间远远小于其他体系,且溶剂交换及超临界干燥过程中的收缩开裂现象明显改善;扫描电镜分析结果显示,硫酸为催化剂制备的Ta2O5气凝胶骨架颗粒间存在较严重的团簇现象,比表面积约167 m2/g,明显低于以盐酸、硝酸为催化剂的体系。X射线光电子能谱测试结果显示,Ta2O5气凝胶中无相应的Cl元素或N元素残留,而S元素则基本上滞留在Ta2O5气凝胶中。说明S元素进入了Ta-O-Ta交联结构,正是因为这种结构的引入,Ta2O5气凝胶的收缩龟裂现象得以明显改善并呈现出相对较高的力学性能。Abstract: Ta2O5 aerogels are prepared by sol-gel technique in the presence of different kinds of acid catalysts such as HCI,HNO3 and H2SO4. The gelation time of H2SO4 system is far less than that of HCI and HNO3 systems. Moreover, the shrinkage and cracking phenomena of Ta2O5 gels in solvent exchnging process and supercritical drying process, which are unavoidable in HCI and HNO3 systems, are obviously inhibited in H2SO4 system. The SEM observations find that the particles of Ta2O5 aerogels catalyzed by H2SO4 are much bigger due to the cluster effect of nano-particles. The BET analysis finds that Ta2O5 aerogels catalyzed by H2SO4 exhibit the BJH surface area of 167 m2/g, which is much lower due to the cluster phenomenon. XPS estimating results reveal that all the S but no CI or N elements remain in Ta2O5 aerogels, indicating that S element is in the Ta-O-Ta crosslinking structure. Due to this particular structure, the shrinkage and cracking phenomena of Ta2O5 aerogels are significantly prevented, and better mechanical properties are achieved.
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Key words:
- acid catalysis /
- ta2o5 aerogel /
- sol-gel /
- hydrolysis
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