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机构地区:[1]上海应用技术大学材料科学与工程学院,上海201418 [2]华东理工大学化工学院,上海200237
出 处:《新型炭材料》2017年第3期258-264,共7页New Carbon Materials
基 金:National Natural Science Foundation of China(50872033,U1332107,U1532105);Fund of Key Laboratory of Carbon Materials,Chinese Academy of Sciences(KFJJ0903);the Capacity Building Program of Shanghai Local Universities(12160503600);First-class Discipline Construction Fund of Shanghai Municipal Education Commission(J201212);Key Discipline Construction Fund of Composite Materials of Shanghai Institute of Technology(10210Q150001)~~
摘 要:用Al(NO_3)_3·9H_2O作为Al_2O_3源,间苯二酚-糠醛为碳源,环氧丙烷为凝胶促进剂,通过溶胶-凝胶方法一釜合成了湿凝胶,并经超临界正己烷干燥和碳化制备了Al_2O_3-C杂化气凝胶。研究了Al_2O_3含量、间苯二酚-糠醛浓度和环氧丙烷/铝摩尔比对所合成的杂化气凝胶孔隙性质的影响。结果表明,此杂化气凝胶均为中孔结构,其平均孔径小于20 nm,Al_2O_3属于γ-型结构但X射线衍射峰很宽。杂化气凝胶在Al_2O_3含量小于5.31 wt%和间苯二酚-糠醛浓度为10 g/mL时可形成整体块状。在其他条件相同的情况下,中孔孔容、BET比表面、外表面积和中孔孔径随环氧丙烷/铝摩尔比增加而增大。制备过程中凝胶的体积收缩率和炭化收率随Al_2O_3含量增加而增大,但密度随Al_2O_3含量增加在4.93 wt%处达到最大。中孔孔容和孔径以及外表面积在环氧丙烷/铝摩尔比为5和6时随间苯二酚-糠醛浓度增加而减小,而在环氧丙烷/铝摩尔比为4时随间苯二酚-糠醛浓度增加而增大。Al2O3 -C hybrid aerogels were prepared by a one-pot sol-gel method,supercritical n-hexane drying and carbonizationusing Al(NO3 ) 3 ,9H2O as the Al2O3 source,resorcinol (R) and furfural (F ) as carbon precursors,and propylene oxide (PO) as a gelation initiator. The effects of the Al2O3 contents,the R+F concentrations and the PAl molar ratios on the porosity of the hy-brid aerogels were investigated using a constant molar ratio of 0. 5. It was found that the hybrid aerogels are all mesoporous with an average pore size below 20 nm. The crystalline structure of Al2O3 is -type,but its diffraction peaks are quite broad. The hybrid aerogels are monolithic when the Al2O3 content is below 5.31 wt% with an R+F concentration of 10 g/100 mL. The meso- pore volume and size,BET surface area and external surface area all increase with increasing PO/Al molar ratio under otherwise identical conditions. The volume shrinkage decreases, carbonization yield increases and the density of the hybrid aerogel exhibits a maximum with an Al2O3 content of 4.93 wt%. The size and volume of the mesopores,and the external surface area decrease with the increasing R+F concentration at PO/Al ratios of 5 and 6,but increase with increasing R+F concentration at a PO/Al ratio of 4.
关 键 词:氧化铝-碳杂化气凝胶 溶胶-凝胶 超临界干燥
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