新型碳铜基纳米结构材料的设计合成及电分析应用研究
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摘要
碳纳米电极材料因具有杰出的优点(在酸碱溶液中稳定，在水溶液中宽的电位窗口，良好的生物相容性，低成本，高的电催化性能)已经成为电分析领域的研究热点。但是关于它的电催化本质还存在很大分歧，因此探讨其催化本质对于设计高性能碳基纳米电极材料具有重要的指导意义。铜纳米电极材料价格低廉，具有能够直接氧化碳水化合物却不造成电极表面污染等特点，是一类非常优秀的电极材料。本文旨在设计合成几种性能优异的新型碳和铜基纳米结构材料，并以其为电极修饰材料，用于灵敏度高、响应迅速、选择性好的电化传感器的研制，考察了这些传感器在医学和环境监测中的应用性能。
论文的第一章不仅详细介绍了碳基、铜基纳米结构材料的合成方法及其在各领域中的应用，而且还对电化学传感器及其环境医学应用进行了简单介绍。论文的第二章以介孔二氧化硅为硬模板，设计并合成了3种不同比表面的纳米孔碳材料。利用氮气吸附、拉曼光谱和透射电镜等技术对这三种纳米孔碳材料进行了详细的结构形貌表征。采用循环伏安和微分脉冲伏安法对比研究了三种材料对抗坏血酸、多巴胺和尿酸的电催化氧化性能。实验结果表明，纳米孔碳材料的比表面越大，缺陷点位越多，催化活性越高。以比表面最高的纳米孔碳为电极材料，研制了同时检测抗坏血酸、多巴胺和尿酸的电化学生物传感器。该传感器灵敏度高，具有潜在的应用价值。在第三章中，以嵌段共聚物(F127)为软模板，合成了介孔碳纳米球。软模板法制备碳材料较硬模板法简单，所合成的介孔碳球的粒径为纳米级，便于制备均一的分散相，更利于分析底物在介孔孔道中的扩散，可望缩短分析物的响应时间，提高分析速度。软模板合成的介孔碳纳米球应用于电化学传感器的研制时，在抗坏血酸、多巴胺和尿酸的同时检测性能方面，获得了令人满意的结果。此外，我们还设计合成了和介孔碳纳米球粒径和孔径大小相似的介孔SiO_2纳米球以及粒径大小相似的碳纳米实心球，以探究介孔碳纳米球的高电催化活性的可能原因。通过对大小相同的三种纳米球材料的微结构形貌表征、电化学及电催化性能的对比，我们认为介孔碳纳米球的高电催化活性，主要归因于介孔碳球内纳米孔的特殊结构---纳米孔的石墨烯壁上含有更多的缺陷点位，这也是抗坏血酸、多巴胺、尿酸可同时检测的主要原因。论文的第四章通过直接高温碳化金属有机骨架化合物，一步获得了氮掺杂纳米碳材料。这种异质原子掺杂的碳纳米结构电极材料不仅能够同时区分抗坏血酸、多巴胺和尿酸的氧化峰，而且还能同时区分邻苯二酚和对苯二酚的氧化峰。以该新型氮掺杂碳纳米结构材料为电极材料，所制备的电化学传感器展现了优异的伏安同时检测性能，在生物医学和环境分析领域可能具有应用前景。在第五章中，我们合成了半有序的介孔碳纳米结构材料，其独特的微结构既展现了快速的电子传输性能，又具有很好的电催化性能。以半有序介孔碳为电极材料，所制备的电化学传感器呈现出了良好的亚硝酸盐检测性能。第六章以廉价的铜片为原料，采用一步液相合成法，获得了氢氧化铜纳米管阵列膜和氧化铜纳米花结构膜。将该氢氧化铜纳米管阵列膜直接做为工作电极，研究了其对葡萄糖电氧化的催化性能。和氧化铜纳米花结构膜的催化性能相比，氢氧化铜纳米管阵列膜具有更好的电催化性能，主要归因于氢氧化铜纳米管特殊的催化活性及其在导电基底表面上的有序排列，上述特点赋予该传感器以快速灵敏的电流响应。在论文第七章中，首先利用表面活性剂十二烷基苯磺酸钠非共价修饰石墨烯表面，获得了分散性良好的功能化石墨烯纳米复合材料；其次，利用功能化石墨烯所具有的良好分散性和高比表面性质，在功能化石墨烯表面电化学生长CuO/Cu复合纳米结构；最后，以表面负载CuO/Cu纳米结构的功能化石墨烯为电极材料，系统考察了果糖的电氧化及分析检测性能。
Carbon nanomaterials have attracted significant interests in the design of electrodes for electroanalysis because of their excellent properties such as electrochemical potential window in aqueous solution, biocompatibility, low-cost, and electrocatalytic activity for a variety of redox reactions, chemical stability in either acidic or basic solution. However, the fundamental reason for the electrochemical activity of carbon material is still controversial. Therefore, an understanding of the fundamental reasons for electrochemical activity of carbon material is vital to design high performance electrochemical devices. Copper-based nanomaterials, one kind of excellent electrode materials, is widely available, inexpensive and can oxidize carbohydrates directly without causing surface contamination. This paper aims at preparing various electrochemical sensors with high sensitivity, fast response and good selectivity by combining carbon-and copper-based nanaomaterials with electrochemical technique for detecting biomolecules and pollutants in the medical and environmental fields.
In Chapter1, the synthesis and application of carbon-and copper-nanomaterials were chiefly introduced. The preparation and application of electrochemical sensors were also briefly introduced. In Chapter2, three templated nanoporous carbons (TNCs) materials with substantial different specific surface area were designed and synthesized by a nanocasting method, in which mesoporous silicates acted as the template. The structures and morphologies of these TNCs were characterized and analyzed in detail by Small-angle XRD diffraction (SAXRD), N2-sorption, Raman spectroscopy and Transmission electron microscope (TEM). The electrochemical properties of the TNCs electrodes were also investigated and compared by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). These experimental results indicated that the higher the specific surface area of TNCs is, the larger amount of edge-plane defect sites contains. The improved performance in simultaneous determination of ascorbic acid (AA), Dopamine (DA), and uric acid (UA) at TNC electrode materials with high specific surface area is anticipated. An electrochemical sensor for simultaneous determination of AA, DA and UA was thus achieved by designing TNCs electrode materials with large specific surface area and defect sites. In Chapter3, the highly ordered mesoporous carbon nanoparticles with spherical morphology were designed and synthesized by using commercial available triblock copolymer Pluronic F127as soft template. Compared with the hard template method, the synthesis route of soft template strategy is simple. In addition, the size of mesoporous carbon sphere is up to nanoscale, which makes it easy to prepare the dispersible phase nanomaterial from the corresponding powder. And its mesoporous structures can enable rapid diffusion of analytes across a large surface area and pore, resulting in reduced response time. Here, an excellent electrochemical sensor was successfully obtained based on the mesoporous carbon nanosphere. It can be used for simultaneous determination of AA, DA, UA in their mixture. In addition, mesoporous SiO2nanosphere with similar pore size and carbon nanosphere without pore were also designed and synthesized, in order to learn the nature of discrimination of AA, DA and UA by mesoporous carbon nanosphere electrode materials. Compared with mesoporous SiO2nanosphere and carbon nanosphere, the high electrochemical property of mesoporous carbon nanosphere was ascribed to the more defective sites possessed, as revealed by microstructural, morphological and electrochemcial characterization. This work may also be valuable for scientists who search for excellent carbon materials for biosensing and electrocatalysis. In Chapter4, a N-doped carbon nanomaterial was one-step prepared through direct carbonization of a metal-organic framework. Heteroatoms (such as nitrogen), which are present in the carbon materials, change the electron donor/acceptor characteristics of carbon depending on their chemical states, thus leading to an enhancement of electrochemical properties. This sensor distinguished not only the oxidation peaks of AA, DA, UA coexisted in body fluid, but also the oxidation peaks of catechol (CC) and hydroquinone (HQ), showing promising application in medical and environmental fields. In Chapter5, hemi-ordered nanoporous carbon (HONC) was obtained from a mesoporous silica template through a nano-replication method. In this nanoporous carbon electode material, the ordered porous structure may serve to promote charge transport, and the disordered porous structure may provide more defect sites for electrochemical reaction. The electrochemical sensor based on HONC material displayed fast, sensitive and well selective determination of NO2-. In Chapter6, vertically aligned arrays of Cu(OH)2nanotubes and CuO nanoflowers were grown directly on the copper substrate via a simple one-step reaction. Without any post-treatment, they were demonstrated directly as electrode materials for electrocatalytic oxidation of glucose. The Cu(OH)2arrays exhibited excellent electrochemical performances for glucose oxidation, presenting a low peak potential, high current, and high current-to-background ratio, even in comparison with the CuO nanoflower films. This sensor is expected to play an important role in the field of blood glucose monitoring. In Chapter7, graphene (GR) sheets were non-covalently functionalized by an anionic surfactant sodium dodecyl benzene sulphonate (SDBS). The SDBS functionalized GR (SDBS/GR) not only exhibits excellent water dispersion but also possesses highly dispersed negative charges, which are favorable to anchoring significant copper cations on the basis of electrostatic self-assembled strategy and producing highly dispersed Cu/CuO catalysts via electrochemistry reduction. Results revealed the distinctly enhanced sensing properties of SDBS/GR/CuO-Cu towards fructose, showing significantly lowered overpotential, ultrafast and ultrasensitive current response in a wide linear range.
论文的第一章不仅详细介绍了碳基、铜基纳米结构材料的合成方法及其在各领域中的应用，而且还对电化学传感器及其环境医学应用进行了简单介绍。论文的第二章以介孔二氧化硅为硬模板，设计并合成了3种不同比表面的纳米孔碳材料。利用氮气吸附、拉曼光谱和透射电镜等技术对这三种纳米孔碳材料进行了详细的结构形貌表征。采用循环伏安和微分脉冲伏安法对比研究了三种材料对抗坏血酸、多巴胺和尿酸的电催化氧化性能。实验结果表明，纳米孔碳材料的比表面越大，缺陷点位越多，催化活性越高。以比表面最高的纳米孔碳为电极材料，研制了同时检测抗坏血酸、多巴胺和尿酸的电化学生物传感器。该传感器灵敏度高，具有潜在的应用价值。在第三章中，以嵌段共聚物(F127)为软模板，合成了介孔碳纳米球。软模板法制备碳材料较硬模板法简单，所合成的介孔碳球的粒径为纳米级，便于制备均一的分散相，更利于分析底物在介孔孔道中的扩散，可望缩短分析物的响应时间，提高分析速度。软模板合成的介孔碳纳米球应用于电化学传感器的研制时，在抗坏血酸、多巴胺和尿酸的同时检测性能方面，获得了令人满意的结果。此外，我们还设计合成了和介孔碳纳米球粒径和孔径大小相似的介孔SiO_2纳米球以及粒径大小相似的碳纳米实心球，以探究介孔碳纳米球的高电催化活性的可能原因。通过对大小相同的三种纳米球材料的微结构形貌表征、电化学及电催化性能的对比，我们认为介孔碳纳米球的高电催化活性，主要归因于介孔碳球内纳米孔的特殊结构---纳米孔的石墨烯壁上含有更多的缺陷点位，这也是抗坏血酸、多巴胺、尿酸可同时检测的主要原因。论文的第四章通过直接高温碳化金属有机骨架化合物，一步获得了氮掺杂纳米碳材料。这种异质原子掺杂的碳纳米结构电极材料不仅能够同时区分抗坏血酸、多巴胺和尿酸的氧化峰，而且还能同时区分邻苯二酚和对苯二酚的氧化峰。以该新型氮掺杂碳纳米结构材料为电极材料，所制备的电化学传感器展现了优异的伏安同时检测性能，在生物医学和环境分析领域可能具有应用前景。在第五章中，我们合成了半有序的介孔碳纳米结构材料，其独特的微结构既展现了快速的电子传输性能，又具有很好的电催化性能。以半有序介孔碳为电极材料，所制备的电化学传感器呈现出了良好的亚硝酸盐检测性能。第六章以廉价的铜片为原料，采用一步液相合成法，获得了氢氧化铜纳米管阵列膜和氧化铜纳米花结构膜。将该氢氧化铜纳米管阵列膜直接做为工作电极，研究了其对葡萄糖电氧化的催化性能。和氧化铜纳米花结构膜的催化性能相比，氢氧化铜纳米管阵列膜具有更好的电催化性能，主要归因于氢氧化铜纳米管特殊的催化活性及其在导电基底表面上的有序排列，上述特点赋予该传感器以快速灵敏的电流响应。在论文第七章中，首先利用表面活性剂十二烷基苯磺酸钠非共价修饰石墨烯表面，获得了分散性良好的功能化石墨烯纳米复合材料；其次，利用功能化石墨烯所具有的良好分散性和高比表面性质，在功能化石墨烯表面电化学生长CuO/Cu复合纳米结构；最后，以表面负载CuO/Cu纳米结构的功能化石墨烯为电极材料，系统考察了果糖的电氧化及分析检测性能。
Carbon nanomaterials have attracted significant interests in the design of electrodes for electroanalysis because of their excellent properties such as electrochemical potential window in aqueous solution, biocompatibility, low-cost, and electrocatalytic activity for a variety of redox reactions, chemical stability in either acidic or basic solution. However, the fundamental reason for the electrochemical activity of carbon material is still controversial. Therefore, an understanding of the fundamental reasons for electrochemical activity of carbon material is vital to design high performance electrochemical devices. Copper-based nanomaterials, one kind of excellent electrode materials, is widely available, inexpensive and can oxidize carbohydrates directly without causing surface contamination. This paper aims at preparing various electrochemical sensors with high sensitivity, fast response and good selectivity by combining carbon-and copper-based nanaomaterials with electrochemical technique for detecting biomolecules and pollutants in the medical and environmental fields.
In Chapter1, the synthesis and application of carbon-and copper-nanomaterials were chiefly introduced. The preparation and application of electrochemical sensors were also briefly introduced. In Chapter2, three templated nanoporous carbons (TNCs) materials with substantial different specific surface area were designed and synthesized by a nanocasting method, in which mesoporous silicates acted as the template. The structures and morphologies of these TNCs were characterized and analyzed in detail by Small-angle XRD diffraction (SAXRD), N2-sorption, Raman spectroscopy and Transmission electron microscope (TEM). The electrochemical properties of the TNCs electrodes were also investigated and compared by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). These experimental results indicated that the higher the specific surface area of TNCs is, the larger amount of edge-plane defect sites contains. The improved performance in simultaneous determination of ascorbic acid (AA), Dopamine (DA), and uric acid (UA) at TNC electrode materials with high specific surface area is anticipated. An electrochemical sensor for simultaneous determination of AA, DA and UA was thus achieved by designing TNCs electrode materials with large specific surface area and defect sites. In Chapter3, the highly ordered mesoporous carbon nanoparticles with spherical morphology were designed and synthesized by using commercial available triblock copolymer Pluronic F127as soft template. Compared with the hard template method, the synthesis route of soft template strategy is simple. In addition, the size of mesoporous carbon sphere is up to nanoscale, which makes it easy to prepare the dispersible phase nanomaterial from the corresponding powder. And its mesoporous structures can enable rapid diffusion of analytes across a large surface area and pore, resulting in reduced response time. Here, an excellent electrochemical sensor was successfully obtained based on the mesoporous carbon nanosphere. It can be used for simultaneous determination of AA, DA, UA in their mixture. In addition, mesoporous SiO2nanosphere with similar pore size and carbon nanosphere without pore were also designed and synthesized, in order to learn the nature of discrimination of AA, DA and UA by mesoporous carbon nanosphere electrode materials. Compared with mesoporous SiO2nanosphere and carbon nanosphere, the high electrochemical property of mesoporous carbon nanosphere was ascribed to the more defective sites possessed, as revealed by microstructural, morphological and electrochemcial characterization. This work may also be valuable for scientists who search for excellent carbon materials for biosensing and electrocatalysis. In Chapter4, a N-doped carbon nanomaterial was one-step prepared through direct carbonization of a metal-organic framework. Heteroatoms (such as nitrogen), which are present in the carbon materials, change the electron donor/acceptor characteristics of carbon depending on their chemical states, thus leading to an enhancement of electrochemical properties. This sensor distinguished not only the oxidation peaks of AA, DA, UA coexisted in body fluid, but also the oxidation peaks of catechol (CC) and hydroquinone (HQ), showing promising application in medical and environmental fields. In Chapter5, hemi-ordered nanoporous carbon (HONC) was obtained from a mesoporous silica template through a nano-replication method. In this nanoporous carbon electode material, the ordered porous structure may serve to promote charge transport, and the disordered porous structure may provide more defect sites for electrochemical reaction. The electrochemical sensor based on HONC material displayed fast, sensitive and well selective determination of NO2-. In Chapter6, vertically aligned arrays of Cu(OH)2nanotubes and CuO nanoflowers were grown directly on the copper substrate via a simple one-step reaction. Without any post-treatment, they were demonstrated directly as electrode materials for electrocatalytic oxidation of glucose. The Cu(OH)2arrays exhibited excellent electrochemical performances for glucose oxidation, presenting a low peak potential, high current, and high current-to-background ratio, even in comparison with the CuO nanoflower films. This sensor is expected to play an important role in the field of blood glucose monitoring. In Chapter7, graphene (GR) sheets were non-covalently functionalized by an anionic surfactant sodium dodecyl benzene sulphonate (SDBS). The SDBS functionalized GR (SDBS/GR) not only exhibits excellent water dispersion but also possesses highly dispersed negative charges, which are favorable to anchoring significant copper cations on the basis of electrostatic self-assembled strategy and producing highly dispersed Cu/CuO catalysts via electrochemistry reduction. Results revealed the distinctly enhanced sensing properties of SDBS/GR/CuO-Cu towards fructose, showing significantly lowered overpotential, ultrafast and ultrasensitive current response in a wide linear range.
引文
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