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尼龙6/碳纳米管复合材料制备及性能研究

Preparation and Studies on Nylon-6/Carbon Nanotubes Composites

作者:李金美
  • 学号
    2001******
  • 学位
    硕士
  • 电子邮箱
    jin******.cn
  • 答辩日期
    2004.06.17
  • 导师
    郭宝华
  • 学科名
    材料科学与工程
  • 页码
    97
  • 保密级别
    公开
  • 馆藏号
    04034056
  • 培养单位
    034 化工系
  • 中文关键词
    尼龙6;碳纳米管;力学性能;结晶性能;电导率
  • 英文关键词
    nylon 6;carbon nanotubes;mechanical properties;crystallization;conductivity

摘要

碳纳米管(CNTs) 具有极高的弹性模量和抗拉强度,并具有独特的导电性能,在高力学强度、高导电性复合材料领域应用前景广阔。近年来聚合物/CNTs复合材料研究发展迅速。本论文选取尼龙6(PA6)/CNTs体系,对复合材料的力学性能、热性能和电性能进行了研究,并对复合材料中CNTs的分散情况、界面性能和复合材料的Raman光谱等进行了表征,在此基础上对复合材料进行了全面的分析。通过考察采用原位复合法、挤出机熔融共混法和共沉淀法制备的三个系列复合材料的力学性能,我们发现共沉淀法得到了性能优良的复合材料。CNTs添加量2wt%时,共沉淀法复合材料拉伸强度比基体提高25%。SEM表明,CNTs含量10wt%时,共沉淀体系未出现团聚现象;样品抽提残留物红外表征发现, CNTs与基体间的界面粘结良好。复合材料的Raman光谱各谱峰均向高波数移动,推测G′峰的蓝移是由于PA6分子紧密包覆CNTs对其造成一定的压应力。DMA表明CNTs含量10wt%时,共沉淀法复合材料Tg比基体提高5.5℃;CNTs含量较高时,复合材料储能模量也较高。TGA表明复合材料的热稳定性略好于基体。CNTs的加入使共沉淀体系结晶度提高6%左右。从CNTs含量5wt%开始,复合材料的结晶曲线在200℃附近出现新峰,并随CNTs含量继续增大峰变大;推测结晶双峰的出现是由于体系在结晶时生成一种晶型与α晶型相同的稳定的结晶相。复合材料电性能良好,添加5wt%(2.8vol%)CNTs,复合材料电导率即达2.1×10-5S/cm;由逾渗理论拟合得出,复合材料的逾渗阈值为3.6wt%;复合材料具有良好的低温和高温NTC效应,说明复合材料具有典型的半导体材料特性; CNTs含量15wt%时,复合材料伏安曲线非线性明显;推测体系的导电机理以场致发射电流为主导。

Carbon nanotubes(CNTs) own outstanding mechanical and electrical properties, thus have promising application in composites fields. Among them, polymer/CNTs composites develop most rapidly these years. In this paper, nylon-6 (PA6)/CNTs composites were prepared by in-situ polymerization, melt-mixing in extruder and co-precipitation process. Mechanical properties, thermal behavior and electrical properties of PA6/CNTs composites were studied, and the dispersion of CNTs in matrix, the interfacial adhesion and Raman spectra etc. were characterized. PA6/CNTs composites made by co-precipitation process were found owning good mechanical properties. With 2wt% CNTs added, the tensile strength of composites improve 25% than the matrix. SEM photos show the uniform dispersion of CNTs in composites made by in-situ polymerization and co-precipitation process. Aggregate are still not found in co-precipitation composites with CNTs content being 10wt%. The interfacial bonding is deduced to be strong by FT-IR spectra. Raman spectrum indicates the peaks of composites shift to high wavenumber compared to original CNTs, maybe owning to the compress stress on the CNTs by the encapsulation of matrix molecules. Tg of composite improves 5.5℃ than the matrix at 10wt% content. Storage modulus increases with increasing CNTs loading. TGA shows the composites possessing better thermal stability than the matrix. The crystallinity of composites improves 6% by CNTs added. A new crystal peak appears at about 200℃ when CNTs content reaches 5wt% and it boosts with increaing CNTs content. The double-humped crystallization procedure is conjectured to be attributed to the emergence of interficial transcrytalline in PA6/CNTs composites. The effection of preparation process and CNTs’ modification on the crystallization behavior were studied.The PA6/CNTs composites as-prepared with high CNTs content were found owning outstanding electrical properties. The conductivity of composites reaches 2.1×10-5 S/cm by merely 5wt%(2.8vol%)CNTs content. The percolation threshold is deduced to be 3.6wt% by percolation theory. The composites present NTC effect both in low temperature and high temperature, indicating their semi-conductor speciality. I-V characteristic of composites behaves super-linear at 15wt% CNTs content. The conducting mechanism of PA6/CNTs composites is presumed to be dominated by field emission current.