氧化石墨烯的功能化及其环氧树脂复合材料的制备与性能研究

发布时间：2018-03-20 15:52

  本文选题：氧化石墨烯　切入点：功能化　出处：《华南理工大学》2015年硕士论文　论文类型：学位论文

【摘要】：本文以三聚氯氰(TCT)、己二胺(HDM)和4,4′-二氨基二苯基甲烷(DDM)为原料,通过调控温度合成出两种带有四个碳氯键的高活性分子TCTHDM和TCTDDM,采用傅立叶红外、核磁共振的方法对合成产物进行了结构表征。然后以氧化石墨烯(GO)为前驱体,通过一步法在表面分别接枝上两种有机小分子TCTHDM和TCTDDM,成功制备出两种功能化氧化石墨烯(TCTHDM-GO和TCTDDM-GO),通过红外光谱、拉曼光谱、X射线衍射、扫描电子显微镜分析了功能化氧化石墨烯的结构和表面形貌,通过热失重分析探究了其热稳定性,并对两种功能化氧化石墨烯的分散性进行了探讨。在接枝上两种小分子后,石墨烯的热稳定性比氧化石墨烯有了提高,片层之间由于引入了有机小分子,无序性和层间距都有所增大。采用非等温DSC法研究了功能化氧化石墨烯对环氧树脂固化行为的影响,随着石墨烯添加量的增大,固化体系达到最大热释放速率的温度越低,固化体系总释放热也越少,而在同一温度下所对应的转化率却越高,分别通过Kissinger和Ozawa两种方法计算了固化反应的活化能,发现比纯环氧树脂的低,说明功能化氧化石墨烯的加入对环氧树脂的固化行为有一定的催化作用。通过热失重分析发现,功能化氧化石墨烯不会改变两种复合材料体系的热分解历程。利用DMA法研究了在不同功能化氧化石墨烯含量下两种固化体系TCTHDM-GO/Epoxy和TCTDDM-GO/Epoxy的储能模量、损耗因子和玻璃化转变温度的变化,发现添加一定量的TCTHDM-GO和TCTDDM-GO能促进环氧树脂交联,提高环氧树脂基体的储能模量及玻璃化转变温度。当添加TCTHDM-GO的质量分数为1.4%时的复合材料,其储能模量达到最大,提高了0.475GPa,而当质量分数为1.0%时,玻璃化转变温度出现极大值,为168.2℃。对于TCTDDM-GO的环氧树脂复合材料,储能模量在质量分数为1.0%处达到最大值,在质量分数为1.4%时,玻璃化转变温度出现极大值,提高了6.5℃。最后,对复合材料的力学性能进行了测试分析,发现少量的功能化氧化石墨烯的加入可提高复合材料的力学性能,拉伸强度最大提升了43%,弯曲强度最大提升了24%,抗冲击强度最大提升了111%。
[Abstract]:In this paper, two kinds of highly active molecules (TCTHDM and TCTDDM) with four carbon-chlorine bonds were synthesized by controlling temperature by using trimelamine, hexanediamine (HDM) and 4Amino-diphenylmethane (DDM) as raw materials, and Fourier transform infrared spectroscopy (FT-IR) was used. The synthesized products were characterized by NMR. Then graphene oxide (GOO) was used as the precursor. Two kinds of functional graphene oxide (TCTHDM-GO) and TCTDDM-GOA (TCTDDM-GOA) were successfully prepared by one-step grafting of two kinds of organic small molecules (TCTHDM and TCTDDM) on the surface, respectively. The two kinds of functionalized graphene oxide TCTHDM-GO and TCTDDM-GOA were prepared by IR, Raman spectra and X-ray diffraction. The structure and surface morphology of functionalized graphene oxide were analyzed by scanning electron microscope (SEM). The thermal stability of functional graphene oxide was investigated by thermogravimetric analysis. The thermal stability of graphene is better than that of graphene oxide. The influence of functionalized graphene oxide on the curing behavior of epoxy resin was studied by non-isothermal DSC method. With the increase of the amount of graphene, the temperature at which the maximum heat release rate of the curing system reached the maximum heat release rate was lower. The lower the total heat release of curing system is, the higher the corresponding conversion is at the same temperature. The activation energy of curing reaction is calculated by Kissinger and Ozawa, respectively, and it is found that the activation energy of curing reaction is lower than that of pure epoxy resin. The results show that the addition of functionalized graphene oxide can catalyze the curing behavior of epoxy resin. The thermal decomposition mechanism of the two composites was not changed by functionalized graphene oxide. The storage modulus of TCTHDM-GO/Epoxy and TCTDDM-GO/Epoxy in two curing systems with different content of graphene oxide were studied by DMA method. With the change of loss factor and glass transition temperature, it is found that adding a certain amount of TCTHDM-GO and TCTDDM-GO can promote the crosslinking of epoxy resin, improve the storage modulus and glass transition temperature of epoxy resin matrix. The storage modulus reached the maximum, increased by 0.475 GPA, and the glass transition temperature reached the maximum of 168.2 鈩，

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