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石墨烯基二维多孔材料的制备及应用研究

发布时间:2018-04-26 15:20

  本文选题:多孔材料 + 二维 ; 参考:《华东理工大学》2015年硕士论文


【摘要】:鉴于石墨烯拥有两种主要的电化学方面的性能:一是石墨烯具有很高的比表面积和优秀的电子传导率,可为离子存储和传输提供理想的平台;二是石墨烯拥有丰富多样的含氧官能团,如氧化石墨烯(GO)和还原氧化石墨烯(RGO)。因此可以作为良好的2D基底,通过负载不同的各向异性生长的金属或金属氧化物纳米颗粒而成为电极材料。近年来,石墨烯及其复合材料已经成为了研究最广泛的电极材料。多孔材料通常具有永久性的多孔性、较低的质量密度、合成的多样化和较高的物理化学稳定性,在气体存储和分离的应用上具有很强的竞争力。本文设计并制备了将多孔材料和石墨烯相结合的复合材料,经过测试,在电催化和气体储存方面显示了优越的性能,本文具体内容为:(1)通过二茂铁(Cp2Fe)和还原石墨烯(rG)的配体交换反应把二茂铁官能团(CpFe)成功的接到还原石墨烯表面上,得到了二茂铁修饰的还原石墨烯(rGFeCp)。用类似的一步反应以二茂铁作为插层剂的石墨片得到了很好的剥离效果,得到了独立的CpFe-基石墨烯纳米片(GFeCp,≈10层)。经过热解和氨气活化后,rGFeCp和GFeCp转化成了二维铁/氮共掺杂多孔石墨烯材料rGFe-800a和GFe-800a。得到的rGFeCp-800a在碱性条件下(0.1MKOH)表现出了很好的氧化还原(ORR)电化学性能,在-0.29 V处出现较低的半波电位,主导四电子转移机制(0.1 V,n=3.5),最大极限扩散电流密度为4.86 mAcm-2。此外,它与20%的商业铂碳相比表现出了极好的耐甲醇性能。铁/氮共掺杂材料将成为具有良好ORR性能材料的重要一员。(2)通过sonogashira连接反应合成三种石墨烯基的共轭二维多孔聚合物高分子(GMP-1,GMP-2和GMP-3),并通过傅里叶变换红外光谱学和固体核磁13CCP/MAS对其化学结构进行确认。在氮气环境下通过热重分析对材料的热稳定性进行测试。利用X射线衍射(XRD)测量GMP系列的结晶性。通过扫描隧道显微镜(SEM)和高分辨率透射电子显微镜(TEM)测量材料的形态和微观结构。在77 K的温度下测量多孔网络N2吸附作用的等温线。相比于其他多孔聚合物,GMP-1、GMP-2和GMP-3的比表面积分别为920m2g-1,636 m2g-1,和211 m2 g-1。得到的孔径分布图表明这些材料具有较窄的孔径分布,分布在1.3至4.0 nm之间。更重要的是,这些多孔高分子表现出了出色的CO2和H2吸收能力。在273 K的温度下,GMP-1的C02的吸收量最多能够达到95.2 mg g-1,属于多孔材料中C02吸收能力最高的一种,H2的吸收能力在77K温度下最多可达113 mg g-1、 GMP-1, GMP-2,和GMP-3的Qst值分别是35,25和21 kJ mol-,相对其他多孔材料要高。高分子网络表现出了对CO2/N2很理想的选择性。以上结果显示了GMP系列材料是可以应用于CO2的存储和分离上有前景的材料。
[Abstract]:Since graphene has two main electrochemical properties: first, graphene has a high specific surface area and excellent electron conductivity, which can provide an ideal platform for ion storage and transport; Second, graphene has rich and diverse oxygen functional groups, such as graphene oxide (GOO) and reduced graphene oxide (RGOG). Therefore, it can be used as a good 2D substrate to form electrode materials by loading different anisotropic metal or metal oxide nanoparticles. In recent years, graphene and its composites have become the most widely studied electrode materials. Porous materials usually have permanent porosity, low mass density, diversity of synthesis and high physical and chemical stability. They are highly competitive in gas storage and separation applications. In this paper, we have designed and prepared composite materials which combine porous materials with graphene. After testing, we have demonstrated excellent performance in electrocatalysis and gas storage. The specific content of this paper is: (1) Ferrocene-modified reduced graphene (rGFeCpN) was prepared by ligand exchange reaction of ferrocene (Cp2Fe2) and reduced graphene (rG). The ferrocene functional group (CpFe2) was successfully connected to the surface of reduced graphene and ferrocene-modified reduced graphene (rGFeCpN) was obtained. The graphite sheet with ferrocene as the intercalation agent has a good peeling effect with a similar one-step reaction, and an independent CpFe- based graphene nanosheet (GFeCp) is obtained, which is about 10 layers. After pyrolysis and ammonia activation, rGFeCp and GFeCp were transformed into two dimensional iron / nitrogen co-doped porous graphene materials rGFe-800a and GFe-800a. The obtained rGFeCp-800a exhibits good electrochemical performance at alkaline condition (0.1 MKOH), with a lower half-wave potential at -0.29 V, leading to a four-electron transfer mechanism of 0.1 V ~ (-1) N ~ (3. 5), and a maximum limiting diffusion current density of 4.86 mAcm-2. In addition, it shows excellent methanol resistance compared with 20% commercial platinum carbon. Iron / nitrogen co-doped material will become an important member of the material with good ORR properties.) three kinds of graphene based conjugated two-dimensional porous polymers, GMP-1, GMP-2 and GMP-3N, will be synthesized by sonogashira bonding reaction. The results of Fourier transform infrared spectroscopy (FTIR) And solid NMR 13CCP/MAS to confirm its chemical structure. The thermal stability of the material was tested by thermogravimetric analysis in nitrogen environment. The crystallinity of GMP series was measured by X-ray diffraction. The morphology and microstructure of the materials were measured by scanning tunneling microscope (SEM) and high resolution transmission electron microscopy (TEM). The isotherm of N 2 adsorption of porous network was measured at 77 K. Compared with other porous polymers, the specific surface areas of GMP-2 and GMP-3 are 920m2g-1636 m2g-1 and 211m2 g-1respectively. The pore size distribution shows that these materials have narrow pore size distribution ranging from 1.3 nm to 4.0 nm. More importantly, these porous polymers exhibit excellent CO2 and H 2 absorption. At 273K, the absorptivity of CO2 of GMP-1 can reach 95.2 mg g ~ (-1) up to 95.2 mg g ~ (-1). The absorption capacity of H _ 2, which belongs to the highest absorption capacity of carbon dioxide in porous materials, can reach 113mg g ~ (-1), GMP-1, GMP-2 and GMP-3 at 77K, respectively. The Qst values of GMP-1 and GMP-3 are 3 525 and 3 525, respectively. 21 kJ mol -, which is higher than other porous materials. Polymer networks exhibit ideal selectivity to CO2/N2. The results show that GMP series are promising materials for CO2 storage and separation.
【学位授予单位】:华东理工大学
【学位级别】:硕士
【学位授予年份】:2015
【分类号】:TB383.4;TQ127.11

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