基于氧化石墨烯和石墨烯的复合凝胶的制备、表征及其应用

发布时间：2018-02-16 19:44

本文关键词： 氧化石墨烯石墨烯聚合物复合水凝胶复合气凝胶　出处：《北京理工大学》2015年硕士论文　论文类型：学位论文

【摘要】：本文阐述了基于氧化石墨烯和石墨烯的复合凝胶材料的制备、表征及其应用。以氧化石墨烯为原材料,通过无催化剂的原位聚合方法制备得到了氧化石墨烯/吡咯甲醛聚合物的复合水凝胶,进一步干燥得到氧化石墨烯/吡咯甲醛聚合物复合气凝胶,对以上水凝胶及气凝胶进行了详细的结构性能表征和气体吸附方面的应用探究。此外,以氮掺杂石墨烯气凝胶为基础,制备了氮掺杂石墨烯/硫复合多孔材料(NGA/S),并研究了硫的引入对氮掺杂石墨烯气凝胶的影响。本文的主要研究内容及结论如下:(1)首先,以吡咯、甲醛单体为原材料,在氧化石墨烯水分散液中通过原位聚合法成功制备了氧化石墨烯/吡咯甲醛聚合物复合水凝胶。分别利用扫描电子显微镜(SEM)、流变测试、X射线衍射(XRD)、X射线光电子能谱(XPS)、激光拉曼(Raman)、近红外光谱(IR)等测试手段对该复合水凝胶的结构、成分、微观形貌等性质进行了表征。通过一系列控制实验证明,在形成凝胶的过程中,氧化石墨烯不仅可以作为模版,而且可以作为催化剂促进聚合物的生成。(2)以氧化石墨烯/吡咯甲醛聚合物的复合水凝胶为前驱体,对其进行冷冻干燥处理,得到相应的氧化石墨烯/吡咯甲醛聚合物的复合气凝胶。通过透射电子显微镜(TEM)进一步观察了该气凝胶的形貌,另外通过N2吸脱附测试对不同比例的氧化石墨烯/吡咯甲醛聚合物的复合气凝胶的孔结构进行了研究分析,发现该气凝胶具有很高的比表面积,最高值达665 m2 g?1。此外,还对不同比例的氧化石墨烯/吡咯甲醛聚合物的复合气凝胶进行了气体吸附测试,结果表明,此类复合气凝胶在273 K下对二氧化碳的吸附量最高可以达到11.1 wt%,在气体吸附应用方面具有优异的性能。(3)最后,以氮掺杂石墨烯气凝胶为基体,将升华硫和氮掺杂石墨烯气凝胶混合物进行热处理,使熔融态的硫渗入氮掺杂石墨烯气凝胶的孔内,制备了氮掺杂石墨烯/硫复合多孔材料。通过SEM、XRD、N2吸脱附测试、XPS、Raman分析了硫的引入对氮掺杂石墨烯气凝胶在孔结构、成分等方面的影响。该复合多孔材料的锂硫电池性能还需进一步研究,期望其能具有优异的锂硫电池性能。
[Abstract]:In this paper, the preparation, characterization and application of composite gel materials based on graphene oxide and graphene oxide are described. The composite hydrogels of graphene oxide / pyrrolidene polymer were prepared by in-situ polymerization without catalyst, and the composite aerogel of graphene oxide / pyrrolidone polymer was further dried. The structure and properties of the hydrogels and aerogels mentioned above were characterized in detail and the application of gas adsorption was explored. In addition, the nitrogen doped graphene aerogels were used as the basis. The nitrogen-doped graphene / sulfur composite porous material was prepared, and the influence of sulfur on the nitrogen-doped graphene aerogel was studied. The main contents and conclusions of this paper are as follows: firstly, pyrrole and formaldehyde monomers are used as raw materials. Graphene oxide / pyrrolidone polymer composite hydrogels were successfully prepared by in-situ polymerization in aqueous graphene oxide dispersion. The X-ray photoelectron energy (XRDX) was measured by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The structure of the composite hydrogel was measured by means of spectral X-ray spectroscopy (XPS), laser Raman Raman spectroscopy (Ram), near infrared spectroscopy (NIR) and so on. Through a series of controlled experiments, it is proved that graphene oxide can not only be used as template in the process of gel formation. Moreover, it can be used as a catalyst to promote the formation of polymers.) the composite hydrogels of graphene oxide / pyrrolidone polymer were used as precursors for freeze-drying treatment. A composite aerogel of graphene oxide / pyrrolidone polymer was obtained. The morphology of the aerogel was further observed by transmission electron microscopy (TEM). In addition, the pore structure of graphene oxide / pyrrole-formaldehyde polymer composite aerogel with different proportion was studied by N2 adsorption and desorption test. It was found that the aerogel had a high specific surface area with a maximum value of 665 m ~ 2 路g ~ (-1)? 1. In addition, the gas adsorption tests of graphene oxide / pyrrolidene polymer composite aerogels with different proportions were carried out. The adsorption capacity of carbon dioxide on the composite aerogels at 273 K is up to 11.1 wt.The composite aerogels have excellent performance in gas adsorption applications. Finally, nitrogen-doped graphene aerogels are used as the matrix. The mixture of sublimated sulfur and nitrogen-doped graphene aerogel was heat-treated, and the molten sulfur was permeated into the pore of nitrogen-doped graphene aerogel. A nitrogen-doped graphene / sulfur composite porous material was prepared. The pore structure of nitrogen-doped graphene aerogels was analyzed by means of XRDN _ 2 adsorption and desorption test. The performance of the composite porous lithium-sulfur battery needs to be further studied, and it is expected that the composite porous material will have excellent lithium-sulfur battery performance.
【学位授予单位】：北京理工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O648.17;TB332

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