溶液剥离石墨烯的制备及其在金属电催化甲醇氧化和增强聚合物上的潜在应用

发布时间：2018-05-10 17:33

本文选题：石墨烯 + 复合材料　；参考：《青岛科技大学》2015年硕士论文

【摘要】：石墨烯以其独特的二维结构和优异的导电、导热和力学等性能,在电子、能源和传感器等领域具有巨大的潜在应用价值。本论文主要研究溶液剥离石墨烯的制备以及它在无机金属电催化甲醇氧化和增强聚合物材料方面的初步应用。主要内容包括以下几部分：1.利用Hummers法和溶液剥离法分别成功地制备了氧化石墨(GO)和溶液剥离石墨烯(PG)。通过傅立叶红外光谱(FT-IR)、X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)和拉曼光谱(Raman)测试手段分别对氧化石墨和溶液剥离石墨烯(PG)的结构和形貌进行表征。结果表明氧化石墨表面含有丰富的含氧官能团,这有利于进一步进行功能化,不过含氧官能团的存在也破坏了石墨上碳原子sp2杂化结构：而溶液剥离石墨烯的含氧官能团少、片层薄同时结构缺陷度低,很好地保留了石墨烯的大π共轭结构。这种溶液剥离石墨烯特别适用于制备高性能无机金属/金属氧化物复合材料和高分子复合材料。2.通过一种简单而有效的超临界流体法成功地把不同摩尔比的铂、镍金属合金纳米粒子负载在炭黑(XC-72)和溶液剥离石墨烯上。通过X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)和拉曼光谱(Raman)测试手段对样品进行表征。结果表明金属合金超细粉粒均匀地分散在超薄石墨烯片层上。通过循环伏安法和计时电流法测试催化剂催化甲醇氧化的活性和稳定性。电化学测试结果揭示,与商业Pt/C和以炭黑为载体的催化剂相比,石墨烯为载体的催化剂催化甲醇氧化的活性和稳定性明显更高。在所有催化剂中,Pt3Ni/PG的催化活性最高。溶液直接剥离的石墨烯为Pt等电化学催化剂的优异载体。这一超临界方法也可拓展到制备其它具有优越性能的金属或金属氧化物／直接剥离石墨烯复合材料。3.采用溶液共混和反溶剂絮凝的方法制备了一系列不同含量的溶液剥离石墨烯／聚苯乙烯复合材料。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、差示扫描量热仪(DSC)和动态力学分析(DMA)等测试手段对样品进行了表征。测试结果表明溶液剥离石墨烯很好地分散在聚苯乙烯基体中；与纯聚苯乙烯相比,石墨烯／聚苯乙烯的热稳定性得到了明显提高。拉伸测试结果显示,石墨烯添加量为0.5wt%时,复合材料的拉伸强度和杨氏模量分别增加了63.5%和77.4%。储能模量的提高也证实溶液剥离石墨烯为聚苯乙烯的理想填料。
[Abstract]:Graphene has great potential applications in electronic, energy and sensor fields for its unique two-dimensional structure and excellent electrical, thermal and mechanical properties. In this paper, the preparation of solution stripping graphene and its preliminary application in inorganic metal electrocatalytic methanol oxidation and reinforced polymer materials were studied. The main content includes the following parts: 1. The Hummers method and the solution stripping method were used to successfully prepare the graphite-oxide (GPO) and the solution-stripping graphene (PGN), respectively. The structure and morphology of graphite oxide and graphene (PGN) were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy (Raman), respectively. The results show that there are abundant oxygen functional groups on the surface of graphite oxide, which is beneficial to further functionalization. However, the existence of oxygen functional groups also destroys the sp2 hybrid structure of carbon atoms on graphite. The large 蟺 conjugate structure of graphene is well preserved because of the thin lamellar and low structural defects. This solution is especially suitable for preparing high performance inorganic metal / metal oxide composites and polymer composites. A simple and effective supercritical fluid method was developed to successfully load platinum and nickel alloy nanoparticles with different molar ratios on carbon black XC-72) and to peel off graphene from the solution. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy (Raman). The results show that ultrafine particles of metal alloy are uniformly dispersed on ultrathin graphene lamellae. The catalytic activity and stability of the catalyst for methanol oxidation were measured by cyclic voltammetry and chronoamperometry. Compared with commercial Pt/C and carbon black supported catalysts, the catalytic activity and stability of graphene supported catalysts for methanol oxidation were significantly higher than those of commercial Pt/C and carbon black supported catalysts. Among all the catalysts, the catalytic activity of Pt3Ni / PG was the highest. Graphene, which is directly stripped from the solution, is an excellent support for Pt and other electrochemical catalysts. This supercritical method can also be extended to the preparation of other metal or metal oxides with superior properties. A series of graphene / polystyrene composites with different contents were prepared by solution blending and antisolvent flocculation. The samples were characterized by means of scanning electron microscope (SEM), transmission electron microscope (TEM), differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). The results showed that graphene was well dispersed in polystyrene matrix and the thermal stability of graphene / polystyrene was obviously improved compared with pure polystyrene. The tensile test results showed that the tensile strength and Young's modulus of the composites increased by 63.5% and 77.4% respectively when the content of graphene was 0.5 wt%. The increase of storage modulus also confirmed that the solution stripping graphene is the ideal filler for polystyrene.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.11

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