石墨烯基纳米薄膜复合材料的制备及在电化学传感器上的应用
发布时间：2019-03-27 08:43
【摘要】：石墨烯(GR)是一种独特二维空间尺寸的纳米材料,具有独特的电学性质、热学性质、机械强度、较大的比表面积、原料易得等特点,近年来引起了科学研究人员的广泛关注。自2004年英国科学家Geim等人首次制备了单层二维片状石墨烯,立即引起了科学界的研究和探索。石墨烯的出现填补了碳家族中二维结构材料的空缺,使得碳纳米材料从零维、一维、二维到三维形成了一个完整的体系。基于石墨烯材料已在光电学、催化储能、传感器等诸多领域的应用。本论文采用优化Hummer法对石墨粉进行化学剥离,得到亲水的氧化石墨烯(graphene oxide,GO)。以氧化石墨烯为前驱体,通过化学合成法制备了基于石墨烯基的复合材料,并对得到的产物性能进行表征;同时通过实验的分析和探讨复合材料的优势并将其用于电化学传感器领域,制备了基于石墨烯基的复合物传感器。其主要内容如下:(1)通过高锰酸钾(KMnO_4)、浓硫酸(H_2SO_4)及硝酸钠(NaNO_3)作氧化剂,对石墨粉进行化学氧化切割,使其表面和边缘修饰上羟基、羧基、环氧等亲水性基团。通过过滤、洗涤、透析等方法,最后将得到氧化石墨烯GO。再以氧化石墨烯(GO)为前驱体与氯化亚铜(CuCl)在碱性溶液下,通过单模微波反应器,形成稳定三维多孔结构的CuO/r-GO复合材料。该复合材料用扫描电镜(SEM),透射电镜(TEM)表征形貌,X射线衍射仪(XRD)表征晶格结构,吸附-脱附等温测试(BET)表征材料的孔隙。CuO/r-GO复合物修饰电极应用于葡萄糖的电化学传感器具有较高的灵敏度和稳定性,宽的线性范围和低的检出限等优点。(2)利用高温加热的方法合成了碳量子点(CDs),再通过化学还原制备了碳量子点功能化的石墨烯(CDs/r-GO)。扫描电镜(SEM),透射电镜(TEM)表征形貌,原子力显微镜(AFM)研究表面结构和厚度,红外光谱(FT-IR)、紫外光谱(UV-vis)和荧光探讨材料的光学特性。由于在CDs和r-GO之间存在强的电子转移,通过层与层之间的π-π堆积和电子之间的转移作用能够加速电子转移,使复合材料具有高的电导性、电催化和氧化还原能力等性能。该复合材料可作为电化学传感器定量分析对苯二酚(HQ)、邻苯二酚(CC)和间苯二酚(RC)。此外,CDs/r-GO/GCE进一步用于实际检测,得到较为满意的效果。(3)硫化镉/还原氧化石墨烯(CdS/r-GO)复合物通过水热反应合成,CdS/r-GO复合物被成功用来检测苯二酚异构体。通过对转移系数(α)和电子迁移速率(ks)等进行了电荷的转移原理的探究,循环伏安法和差分脉冲伏安法等测试了CdS/r-GO复合物的电化学性能。此外,该传感器成功的对苯二酚异构体进行定量检测,进一步的实际应用也得到满意的效果。
[Abstract]:Graphene (GR) is a kind of special two-dimensional space-size nanomaterials with unique electrical properties, thermal properties, mechanical strength, large specific surface area, easy availability of raw materials, and so on. In recent years, it has attracted wide attention of scientific researchers. Single-layer two-dimensional flake graphene has been prepared for the first time by British scientist Geim et al in 2004, which has aroused the scientific research and exploration immediately. The appearance of graphene fills the gap of two-dimensional structural materials in the carbon family, which makes the carbon nanomaterials form a complete system from zero-dimensional, one-dimensional, two-dimensional to three-dimensional. Graphene-based materials have been applied in many fields such as photoelectricity, catalytic energy storage, sensors and so on. In this paper, the hydrophilic graphene oxide (graphene oxide,GO) was obtained by chemical stripping of graphite powder by optimized Hummer method. Graphene-based composites were prepared by chemical synthesis using graphene oxide as precursor and their properties were characterized. At the same time, the advantages of the composites were analyzed experimentally and applied to the field of electrochemical sensors, and the composite sensors based on graphene group were prepared. The main contents are as follows: (1) by using potassium permanganate (KMnO_4), concentrated sulfuric acid (H_2SO_4) and sodium nitrate (NaNO_3) as oxidants, the graphite powder was chemically oxidized to modify the hydroxyl and carboxyl groups on its surface and edge. Hydrophilic groups such as epoxy. Finally, graphene oxide GO. can be obtained by filtration, washing, dialysis, etc. Then, using graphene oxide (GO) as precursor and cuprous chloride (CuCl) in alkaline solution, a stable three-dimensional porous CuO/r-GO composite was formed through a single-mode microwave reactor. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM), and the lattice structure was characterized by X-ray diffraction (XRD). Adsorption-desorption isotherms were used to characterize the pores of the material by (BET). The CuO/r-GO complex modified electrode has high sensitivity and stability when applied to the electrochemical sensor of glucose. The advantages of wide linear range and low detection limit were obtained. (2) carbon quantum dots (CDs),) were synthesized by high temperature heating and then functionalized graphene (CDs/r-GO) was prepared by chemical reduction. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM). The surface structure and thickness were studied by atomic force microscopy (AFM). The optical properties of the materials were investigated by infrared spectroscopy (FT-IR), ultraviolet spectroscopy (UV-vis) and fluorescence. Due to the strong electron transfer between CDs and r-GO, the electron transfer can be accelerated by 蟺-蟺 stacking and electron transfer between layers, which makes the composites have high conductivity. Electrocatalysis and redox ability. The composite can be used as electrochemical sensor for quantitative analysis of hydroquinone (HQ), catechol (CC) and resorcinol (RC). In addition, CDs/r-GO/GCE was further applied to the detection of cadmium sulfide / reduced graphene oxide (CdS/r-GO). (3) cadmium sulfide / reduced graphene oxide (CdS/r-GO) composite was synthesized by hydrothermal reaction. The CdS/r-GO complex was successfully used to detect the isomers of catechol. The charge transfer principle was investigated by the transfer coefficient (伪) and electron transfer rate (ks). The electrochemical properties of CdS/r-GO complex were tested by cyclic voltammetry and differential pulse voltammetry. In addition, the sensor has been successfully used for the quantitative detection of hydroquinone isomers, and its further practical application has also achieved satisfactory results.
【学位授予单位】：闽南师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.1
[Abstract]:Graphene (GR) is a kind of special two-dimensional space-size nanomaterials with unique electrical properties, thermal properties, mechanical strength, large specific surface area, easy availability of raw materials, and so on. In recent years, it has attracted wide attention of scientific researchers. Single-layer two-dimensional flake graphene has been prepared for the first time by British scientist Geim et al in 2004, which has aroused the scientific research and exploration immediately. The appearance of graphene fills the gap of two-dimensional structural materials in the carbon family, which makes the carbon nanomaterials form a complete system from zero-dimensional, one-dimensional, two-dimensional to three-dimensional. Graphene-based materials have been applied in many fields such as photoelectricity, catalytic energy storage, sensors and so on. In this paper, the hydrophilic graphene oxide (graphene oxide,GO) was obtained by chemical stripping of graphite powder by optimized Hummer method. Graphene-based composites were prepared by chemical synthesis using graphene oxide as precursor and their properties were characterized. At the same time, the advantages of the composites were analyzed experimentally and applied to the field of electrochemical sensors, and the composite sensors based on graphene group were prepared. The main contents are as follows: (1) by using potassium permanganate (KMnO_4), concentrated sulfuric acid (H_2SO_4) and sodium nitrate (NaNO_3) as oxidants, the graphite powder was chemically oxidized to modify the hydroxyl and carboxyl groups on its surface and edge. Hydrophilic groups such as epoxy. Finally, graphene oxide GO. can be obtained by filtration, washing, dialysis, etc. Then, using graphene oxide (GO) as precursor and cuprous chloride (CuCl) in alkaline solution, a stable three-dimensional porous CuO/r-GO composite was formed through a single-mode microwave reactor. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM), and the lattice structure was characterized by X-ray diffraction (XRD). Adsorption-desorption isotherms were used to characterize the pores of the material by (BET). The CuO/r-GO complex modified electrode has high sensitivity and stability when applied to the electrochemical sensor of glucose. The advantages of wide linear range and low detection limit were obtained. (2) carbon quantum dots (CDs),) were synthesized by high temperature heating and then functionalized graphene (CDs/r-GO) was prepared by chemical reduction. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM). The surface structure and thickness were studied by atomic force microscopy (AFM). The optical properties of the materials were investigated by infrared spectroscopy (FT-IR), ultraviolet spectroscopy (UV-vis) and fluorescence. Due to the strong electron transfer between CDs and r-GO, the electron transfer can be accelerated by 蟺-蟺 stacking and electron transfer between layers, which makes the composites have high conductivity. Electrocatalysis and redox ability. The composite can be used as electrochemical sensor for quantitative analysis of hydroquinone (HQ), catechol (CC) and resorcinol (RC). In addition, CDs/r-GO/GCE was further applied to the detection of cadmium sulfide / reduced graphene oxide (CdS/r-GO). (3) cadmium sulfide / reduced graphene oxide (CdS/r-GO) composite was synthesized by hydrothermal reaction. The CdS/r-GO complex was successfully used to detect the isomers of catechol. The charge transfer principle was investigated by the transfer coefficient (伪) and electron transfer rate (ks). The electrochemical properties of CdS/r-GO complex were tested by cyclic voltammetry and differential pulse voltammetry. In addition, the sensor has been successfully used for the quantitative detection of hydroquinone isomers, and its further practical application has also achieved satisfactory results.
【学位授予单位】：闽南师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.1
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