溶胶-凝胶一釜法Al<sub>2</sub>O<sub>3</sub>-C杂化气凝胶的合成和表征

张睿; 蒋宁; 段晓佳; 金双玲; 金鸣林

doi:10.1016/S1872-5805(17)60122-7

溶胶-凝胶一釜法Al₂O₃-C杂化气凝胶的合成和表征

doi: 10.1016/S1872-5805(17)60122-7

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

基金项目: 国家自然科学基金（50872033， U1332107， U1532105）；中国科学院炭材料重点实验室基金（KFJJ0903）；上海市地方高校能力建设项目（12160503600），上海市教委一流学科建设计划（J201212）；上海应用技术大学复合材料校级重点建设项目（10210Q150001）.

详细信息

通讯作者:
张睿,教授.E-mail:zhangrui@sit.edu.cn

中图分类号: TB333
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- 被引次数: 0
出版历程
- 收稿日期: 2017-01-08
- 录用日期: 2017-06-28
- 修回日期: 2017-04-30
- 刊出日期: 2017-06-28

Synthesis and characterization of Al₂O₃-C hybrid aerogels by a one-pot sol-gel method

1.
School of Materials Sciences and Engineering, Shanghai Institute of Technology, Shanghai 201418, China;
2.
Chemical Engineering College, East China University of Science and Technology, Shanghai 200237, China

Funds: 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

摘要: 用Al（NO₃）₃·9H₂O作为Al₂O₃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Al₂O₃-C杂化气凝胶。研究了Al₂O₃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，Al₂O₃属于γ-型结构但X射线衍射峰很宽。杂化气凝胶在Al₂O₃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Al₂O₃含量增加而增大，但密度随Al₂O₃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。
- 氧化铝-碳杂化气凝胶 /
- 溶胶-凝胶 /
- 超临界干燥
Abstract: Al₂O₃-C hybrid aerogels were prepared by a one-pot sol-gel method,supercritical n-hexane drying and carbonization using 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 PO/Al molar ratios on the porosity of the hybrid aerogels were investigated using a constant R/F 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 γ-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 mesopore 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.
- Al₂O₃-C hybrid aerogel /
- Sol-gel method /
- Supercritical drying

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