物理化学学报 >> 2015, Vol. 31 >> Issue (6): 1179-1185.doi: 10.3866/PKU.WHXB201504146

材料物理化学 上一篇    下一篇

化学改性氧化石墨烯交联的聚酰亚胺气凝胶

梁祎, 卢赟, 姚维尚, 张学同   

  1. 北京理工大学材料科学与工程学院, 北京100081
  • 收稿日期:2014-12-30 修回日期:2015-04-13 发布日期:2015-06-05
  • 通讯作者: 卢赟, 张学同 E-mail:luyun@bit.edu.cn;zhangxtchina@yahoo.com
  • 基金资助:

    国家自然科学基金(21373024)和北京理工大学创新项目基金资助

Polyimide Aerogels Crosslinked with Chemically Modified Graphene Oxide

LIANG Yi, LU Yun, YAO Wei-Shang, ZHANG Xue-Tong   

  1. School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, P. R. China
  • Received:2014-12-30 Revised:2015-04-13 Published:2015-06-05
  • Contact: LU Yun, ZHANG Xue-Tong E-mail:luyun@bit.edu.cn;zhangxtchina@yahoo.com
  • Supported by:

    The project was supported by the National Natural Science Foundation of China (21373024) and Innovation Program of the Beijing Institute of Technology, China.

摘要:

聚酰亚胺(PI)气凝胶是一类密度低、机械性能好、隔热性能优异的多孔材料, 通常使用昂贵的化学交联剂进行交联. 氧化石墨烯(GO)是近年来广受关注的用于聚合物增强的纳米功能填料. 以前报道的PI/GO 复合材料多是纤维或膜的形式. 为了获得PI/GO 复合气凝胶, 本文采用化学改性氧化石墨烯(m-GO)替代1,3,5-三(4-氨基苯氧基)苯(TAB)等常规的交联剂, 使之与4,4'-二氨基二苯基醚(ODA)和3,3',4,4'-联苯四羧酸二酐(BPDA)反应, 制得了m-GO交联的PI 气凝胶. GO的化学改性通过其与过量ODA在水热条件下反应实现. 通过扫描电子显微镜(SEM)研究了PI/m-GO气凝胶的微观结构. 分别通过氮气吸脱附测试、热重分析和热线法研究了m-GO对气凝胶的孔特性、热稳定性和热导率的影响. 测试结果表明, 所获得的PI/m-GO气凝胶保持了高的孔隙率、热稳定性和绝热性. 压缩测试结果显示, 与采用1.8% (质量分数, w)的TAB进行交联的PI 气凝胶相比,仅用0.6% (w)的m-GO交联所获得的气凝胶具有更高的比杨氏模量(杨氏模量/密度)、比屈服强度(屈服强度/密度)和更小的体积收缩率.

关键词: 聚酰亚胺气凝胶, 氧化石墨烯, 交联, 机械性能, 收缩率

Abstract:

Polyimide (PI) aerogels, which are generally crosslinked using expensive chemical crosslinking agents, are novel porous materials with high strength, high heat resistance, high porosity, and low density. Graphene oxide (GO) is a functional nanofiller that has aroused wide interest in recent years. The reported PI/ GO composites have mostly been in the form of fibers and films. In this study, PI/GO composite aerogels were obtained using chemically modified graphene oxide (m-GO) as the crosslinking agent, instead of traditional ones such as 1,3,5-triaminophenoxybenzene (TAB), by reaction with 4,4'-oxydianiline (ODA) and 3,3',4,4'- biphenyltetracarboxylic dianhydride (BPDA). The chemical modification of GO was achieved by reacting GO with excess ODA using a hydrothermal method. The microstructures of the PI/m-GO aerogels were investigated using scanning electron microscopy (SEM). Nitrogen sorption tests, thermogravimetric analysis, and a hot-wire method were used to investigate the effects of m-GO on the pore properties, thermal stabilities, and thermal conductivities, respectively, of the resulting aerogels. The results show that the PI/m-GO aerogels are highly porous, thermally stable, and heat insulating. Compression tests showed that the PI aerogel prepared using 0.6% (mass fraction, w) m-GO instead of 1.8% (w) TAB as the crosslinking agent had a higher specific Young's modulus [Young's modulus/density (ρ)] and specific yield strength (yield strength/ρ), and less shrinkage.

Key words: Polyimide aerogel, Graphene oxide, Crosslinking, Mechanical property, Shrinkage ratio

MSC2000: 

  • O648