石墨烯及其氧化物复合结构气相沉积法制备研究

发布时间：2018-02-14 19:38

本文关键词： 石墨烯石墨烯基制备装置有序孔复合结构氧化物薄膜　出处：《吉林大学》2017年博士论文　论文类型：学位论文

【摘要】：石墨烯是近年来发现的一种二维碳原子晶体,由六边形网状结构碳原子构成,原子之间结构的排列与石墨单原子层排列相同,它有着非常好的结晶性,是组成其它碳质材料不同维数的基本单元。其C-C之间以SP2键相连,具有大的比表面积。由于其具有独特的电子、光学、力学、热学性质而成为多个学科研究的热门材料,这些性质使石墨烯有着广阔的研究前景和巨大的可用价值,其在各个领域的也存在着极大的潜在应用。为了使石墨烯可以很大程度上的应用于多个领域中,成功有效的制备高质量的石墨烯成为了近年来很多人研究的热点。而化学气相沉积这种相对于其他制备石墨烯方法有很多优势的制备方法,被越来越多的研究者尝试和采用。为了更好探索石墨烯及其氧化物复合结构气相沉积法制备和其性能,本论文首先通过化学气相沉积法对石墨烯薄膜进行制备以及对他的各方面性能进行了探索。采用沉积系统低温沉积石墨烯薄膜,并采用旋涂、转移等方法进行目标基底转移,并对其进行表征。基于原有CVD法制备石墨烯薄膜设备存在的缺点和不足,在详细了解和熟练掌握实验原理及实验操作的基础之上,对原有装置进行研发和改造。通过对各部分组件进行添加、改造和连接,在温区的可控、电极控制和对气体的控制等方面进行实施,努力构造一套完整有序的化学气相沉积系统。其改造组件覆盖腔室内外部、连接操控面板及系统整体。通过示意图及实物图详细描述各部分改造组件的具体构成及连接方式。并利用该系统进行石墨烯薄膜的制备。利用磁控溅射手段,在已经制取的石墨烯表面生长一层氧化物,并对复合薄膜的性能进一步的研究。在ITO表面沉积WO_3薄膜,通过XRD观察WO_3薄膜的结晶度,利用扫描电镜对WO_3的表面形貌进行表征,用CorrTest测试系统进行电致变色性能的研究。采用石英振荡器和台阶仪对WO_3薄膜的厚度进行测量,并用光纤光谱仪对所制取的所制WO_3薄膜的透射率进行测试,对比在350nm-800nm波长范围内的透过率差。通过介绍AAO模板的形成机理和具体应用,详细说明在实验室条件下AAO模板的制备过程。利用两次阳极氧化法制备出规则的正六边形孔状结构。对比了不同实验条件下所制备的AAO模板的区别,包括实验过程中氧化的次数以及对最终制得模板的扩孔时间。为了制备石墨烯基氧化物有序孔结构复合材料,首先利用CVD法进行石墨烯薄膜生长以及石墨烯薄膜的转移。努力探索磁控溅射方法对不同氧化物的制备、在石墨烯基底上的沉积和在有序孔结构中的生长。
[Abstract]:Graphene is a kind of two-dimensional carbon atom crystal found in recent years. It is composed of hexagonal carbon atoms with network structure. The arrangement of atomic structure is the same as that of graphite monatomic layer, and it has very good crystallinity. C-C is the basic unit of different dimensions of other carbonaceous materials. Its C-C is connected by SP2 bond and has a large specific surface area. Because of its unique electronic, optical, mechanical and thermal properties, C-C has become a hot material in many disciplines. These properties make graphene have a broad research prospect and great available value, and it also has great potential applications in various fields. In order to make graphene can be used in many fields to a large extent, The successful and effective preparation of high quality graphene has become a hot topic in recent years, and chemical vapor deposition (CVD), which has many advantages over other methods of graphene preparation, In order to better explore the preparation and properties of graphene and its oxide composite structure by vapor deposition, In this paper, graphene thin films were prepared by chemical vapor deposition (CVD) and their properties were investigated. The graphene thin films were deposited at low temperature in the deposition system, and the target substrates were transferred by spin-coating and transfer methods. Based on the shortcomings and shortcomings of the original CVD equipment for the preparation of graphene thin films, the principle and operation of the experiments are understood and mastered in detail. Through the addition, modification and connection of various components, the control of temperature zone, electrode control and gas control are carried out. Strive to construct a complete and orderly chemical vapor deposition system. The modified components cover the interior and exterior of the chamber, Connecting the control panel and the whole system. The concrete composition and connection mode of each part of the modified module are described in detail by means of schematics and physical diagrams. The graphene film is prepared by using the system, and the magnetron sputtering method is used to prepare the graphene film. A layer of oxide was grown on the surface of the prepared graphene, and the properties of the composite film were further studied. The crystallinity of WO_3 film was observed by XRD, and the surface morphology of WO_3 was characterized by scanning electron microscope (SEM). The electrochromic properties of WO_3 films were studied by CorrTest measurement system. The thickness of WO_3 films was measured by quartz oscillator and step meter, and the transmittance of WO_3 films was measured by optical fiber spectrometer. The difference in transmittance in the wavelength range of 350 nm to 800 nm is compared. The formation mechanism and application of AAO template are introduced. The preparation process of AAO templates under laboratory conditions was described in detail. Regular hexagonal pore structures were prepared by two anodization methods. The differences of AAO templates prepared under different experimental conditions were compared. Including the number of times of oxidation during the experiment and the time of pore expansion for the final template. In order to prepare graphene based oxide ordered pore structure composite, Firstly, the growth of graphene thin films and the transfer of graphene films were carried out by CVD method, and the preparation of different oxides, deposition on graphene substrates and growth in ordered pore structures by magnetron sputtering were explored.
【学位授予单位】：吉林大学
【学位级别】：博士
【学位授予年份】：2017
【分类号】：O613.71;O484

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