石墨烯复合结构的吸附和电催化性能研究
摘要
SP2杂化的碳原子以六角形蜂窝状有序排列形成的二维结构被称为石墨烯。由于其独特的结构特征,石墨烯具有比其它碳类材料更优异的物理和化学性质。例如,单层石墨烯在可见光范围内对光的透过率超过97%,并具有很高的载流子迁移率,使其在透明导电薄膜方面具有广泛的应用空间。石墨烯还有非常大的比表面积,可作为载体支撑物有效地分散各种纳米材料和团簇结构,从而获得各种石墨烯-纳米颗粒和石墨烯-团簇的复合物。这些复合物不但拥有原先单体各自的物理化学特性,同时还具有特殊的增效协同作用,从而进一步拓宽了石墨烯及其复合体系的应用范围,有望在燃料电池的催化、水污染处理、光电探测、锂离子电池等诸多领域展现其迷人的色彩。因此,如何高效制备高质量的石墨烯,如何根据应用目标设计和合成具有集成和协同功能的复合结构,如何提升复合结构的性能等都是人们十分关注的问题。本论文侧重围绕石墨烯及其复合纳米结构的设计和制备及其在污染处理、催化反应的应用等方面开展相关应用基础研究,主要内容分述如下。
在第一章中,我们简要介绍了石墨烯基本的物理和化学性质,总结和比较了石墨烯的各种制备方法及其利弊,同时也对石墨烯-纳米颗粒和石墨烯-团簇复合体系的研究现状做了概述。
在第二章中,我们介绍了一种室温下利用锌粉绿色还原氧化石墨烯(GO)得到还原石墨烯(RGO)的新方法。我们对RGO的还原程度、结构和性质进行了系统的X射线衍射、紫外吸收光谱、拉曼光谱、透光率和电学特性等表征。结果表明：通过调控反应时间,RGO中的碳氧比可从原先的1.67上升到13.7；Zn粉还原的RGO比其它化学还原试剂制备的RGO具有更高的电导率,可达2.7×104s.m-1；厚度20nm的RGO薄膜在450nm到1500nm的波长范围内透光率保持在70%以上,且面电阻仅为2kΩ。这种还原方法价格便宜、环境友好且产量高,所制备的RGO透明导电薄膜有望在光伏、光电以及电化学等领域得到广泛应用。
在第三章中,我们通过简便的化学方法制备了一系列具有不同配比的RGO-Fe3O4纳米复合结构。通过实时监控有机染料分子紫外吸收光谱强度的变化,系统地研究了该复合体系作为吸附剂对多种有机染料分子的吸附机理。结果表明,复合结构中RGO的表面以及Fe304纳米颗粒的磁性使得该复合结构不但对有机染料分子具有非常好的吸附能力,而且可在外磁场的作用下从水溶液中被快速地分离回收。通过简单的退火,复合结构显示出良好的再生作用,其吸附能力也没有明显降低。此外,该复合结构能够在不同的酸碱pH环境以及不同的浓度下,仍保持优良的吸附性能。在混有多种染料的溶液中,复合结构仍表现出与对单一染料分子相同的吸附能力。如此优异的性能使RGO-Fe3O4纳米复合结构材料有望作为一种很好的吸附除污剂,在水污染的治理过程中发挥作用。
在第四章中,我们首次在水溶液中合成得到RGO-Pd团簇复合结构。TEM/HRTEM以及XRD表征表明复合结构中存在大小约为2nm的非晶相Pd金属团簇,这些团簇能够均匀分散在还原石墨烯的表面。通过对照实验,我们证明了氨水的螯合作用可以使氨分子与Pd2+形成络合物Pd(NH3)42+,借助电荷相互作用,这一络合物能够有效吸附在GO表面,并通过高压汞灯的照射还原形成RGO-Pd团簇复合结构。通过对甲酸的催化氧化实验,我们证明了RGO-Pd团簇复合结构不但比RGO-Pd纳米颗粒复合结构具有更强的催化活性,同时也具有更高的催化稳定性,这些结果表明石墨烯金属团簇复合结构有望作为新的催化剂,在燃料电池等领域得到应用。
Graphene, a kind of2-Dimentional nanostructure with sp2carbon atoms in a honeycomb lattice, has more exceptional physical and chemical properties than other carbon materials due to its unique structure. Due to its high transparency over97%in the visible range and ultrahigh carrier mobility, it is a very promising candidate for the transparent conductive films. The graphene is frequently used as a matrix for the nanocomposites, because it has large specific surface area to disperse different nanoparticles and clusters. The produced nanocomposites possess not only both functions of pure graphene and the nanoparticle/cluster, but also some extraordinary synergetic effects, which can probably be utilized widely for fuel cells, water pollutant removal, photodetector and lithium ion batteries. Despite of many remarkable progresses made on the graphene, there is plenty of room for the rational design and controllable synthesis of graphene and its nonocomposite, as well as the spread of their application. Hence, we focused on our attention to the design, synthesis and properties of the graphene and its nanocomposite. The main contents of the dissertation can be summarized as follows:
In chapter one, we reviewed the structure, properties and the synthesis strategies of the graphene. The status of the graphene-nanoparticles and the graphene-cluster was also briefly introduced. The motivation of our research is outlined.
In chapter two, we report a simple, eco-friendly, and high-efficient approach to synthesize reduced graphene oxide (RGO) nanosheets at room temperature based on Zn reduction of exfoliated GO. The evolution of GO to RGO has been characterized by X-ray diffraction, UV-vis absorption spectroscopy and Raman spectroscopy. The results of X-ray photoelectron spectroscopy reveal that the atomic ration of carbon to oxygen in the RGO can be tuned from1.67to13.7through controlling the reduction time. The electrical measurement shows the conductivity of the RGO to be2.7x104s.m-1, much larger than those previously obtained by chemical reduction through other reducing agents. More importantly, the sheet resistance of the RGO film with20nm thickness can be as low as2kΩ, while a high transparency over70%with a broad spectral range from450nm to1500nm can be retained, demonstrating that the produced thin RGO film can be used as a transparent electrode material in a variety of potential application fields such as optoelectronics, photovoltaics and electrochemistry.
In chapter three, a function nanocomposites of RGO-Fe3O4nanoparticles has been chemically synthesized with tunable RGO/Fe3O4ratio. The adsorption behaviors of a series of dyes using these nanocomposites as the adsorbent are systematically investigated through real-time monitoring of the fingerprint spectral changes of the dyes. The results show that, benefiting both from the surface property of RGO and from the magnetic property of Fe3O4, the nanocomposites possess quite a good adsorption capacity to the dyes, and can be easily and rapidly extracted from water by magnetic attraction. Most importantly, it is found that by simply annealing in moderate conditions, this adsorbent can be easily and efficiently regenerated for reuse with hardly any compromise of the adsorption capacity. Furthermore, the adsorbability of this adsorbent shows satisfactory tolerance against the variations in both pH environment and dye concentration. Even when exposed to a multi dye cocktail, this adsorbent can work well without suppressing the adsorption capacity for each of the dyes, as compared with that measured separately. The RGO-Fe3O4nanocomposites with many excellent abilities can be as a promising candidate for highly-efficient dye pollutant removal.
In chapter four, we, for the first time, reported the successful synthesis of RGO-Pd cluster nanocomposite in water solution. HRTEM/TEM and XRD measurements reveal that the nanocomposites contain amorphous Pd clusters with the size of2nm on the matrix of RGO. Based on the results of a serious of control experiments, we proposed the possible mechanism for the preparation of nanocomposite as following. The Pd2+is first coordinated by NH3effectively to form Pd(NH3)42+, and then the Pd(NH3)42+can adsorb onto the GO surface through opposite charges interaction, whereafter both GO and Pd2+will be reduced to form the RGO-Pd cluster nanocomposite under the irradiation of high pressure mercury lamp. Compared to the RGO-PdNPs, the RGO-Pd cluster nanocomposites holds higher catalytic activity and stability for the oxygen reduction reaction of formic acid under the same conditions, making the RGO-Pd cluster as a good new catalyst for fuel cell.
在第一章中,我们简要介绍了石墨烯基本的物理和化学性质,总结和比较了石墨烯的各种制备方法及其利弊,同时也对石墨烯-纳米颗粒和石墨烯-团簇复合体系的研究现状做了概述。
在第二章中,我们介绍了一种室温下利用锌粉绿色还原氧化石墨烯(GO)得到还原石墨烯(RGO)的新方法。我们对RGO的还原程度、结构和性质进行了系统的X射线衍射、紫外吸收光谱、拉曼光谱、透光率和电学特性等表征。结果表明：通过调控反应时间,RGO中的碳氧比可从原先的1.67上升到13.7；Zn粉还原的RGO比其它化学还原试剂制备的RGO具有更高的电导率,可达2.7×104s.m-1；厚度20nm的RGO薄膜在450nm到1500nm的波长范围内透光率保持在70%以上,且面电阻仅为2kΩ。这种还原方法价格便宜、环境友好且产量高,所制备的RGO透明导电薄膜有望在光伏、光电以及电化学等领域得到广泛应用。
在第三章中,我们通过简便的化学方法制备了一系列具有不同配比的RGO-Fe3O4纳米复合结构。通过实时监控有机染料分子紫外吸收光谱强度的变化,系统地研究了该复合体系作为吸附剂对多种有机染料分子的吸附机理。结果表明,复合结构中RGO的表面以及Fe304纳米颗粒的磁性使得该复合结构不但对有机染料分子具有非常好的吸附能力,而且可在外磁场的作用下从水溶液中被快速地分离回收。通过简单的退火,复合结构显示出良好的再生作用,其吸附能力也没有明显降低。此外,该复合结构能够在不同的酸碱pH环境以及不同的浓度下,仍保持优良的吸附性能。在混有多种染料的溶液中,复合结构仍表现出与对单一染料分子相同的吸附能力。如此优异的性能使RGO-Fe3O4纳米复合结构材料有望作为一种很好的吸附除污剂,在水污染的治理过程中发挥作用。
在第四章中,我们首次在水溶液中合成得到RGO-Pd团簇复合结构。TEM/HRTEM以及XRD表征表明复合结构中存在大小约为2nm的非晶相Pd金属团簇,这些团簇能够均匀分散在还原石墨烯的表面。通过对照实验,我们证明了氨水的螯合作用可以使氨分子与Pd2+形成络合物Pd(NH3)42+,借助电荷相互作用,这一络合物能够有效吸附在GO表面,并通过高压汞灯的照射还原形成RGO-Pd团簇复合结构。通过对甲酸的催化氧化实验,我们证明了RGO-Pd团簇复合结构不但比RGO-Pd纳米颗粒复合结构具有更强的催化活性,同时也具有更高的催化稳定性,这些结果表明石墨烯金属团簇复合结构有望作为新的催化剂,在燃料电池等领域得到应用。
Graphene, a kind of2-Dimentional nanostructure with sp2carbon atoms in a honeycomb lattice, has more exceptional physical and chemical properties than other carbon materials due to its unique structure. Due to its high transparency over97%in the visible range and ultrahigh carrier mobility, it is a very promising candidate for the transparent conductive films. The graphene is frequently used as a matrix for the nanocomposites, because it has large specific surface area to disperse different nanoparticles and clusters. The produced nanocomposites possess not only both functions of pure graphene and the nanoparticle/cluster, but also some extraordinary synergetic effects, which can probably be utilized widely for fuel cells, water pollutant removal, photodetector and lithium ion batteries. Despite of many remarkable progresses made on the graphene, there is plenty of room for the rational design and controllable synthesis of graphene and its nonocomposite, as well as the spread of their application. Hence, we focused on our attention to the design, synthesis and properties of the graphene and its nanocomposite. The main contents of the dissertation can be summarized as follows:
In chapter one, we reviewed the structure, properties and the synthesis strategies of the graphene. The status of the graphene-nanoparticles and the graphene-cluster was also briefly introduced. The motivation of our research is outlined.
In chapter two, we report a simple, eco-friendly, and high-efficient approach to synthesize reduced graphene oxide (RGO) nanosheets at room temperature based on Zn reduction of exfoliated GO. The evolution of GO to RGO has been characterized by X-ray diffraction, UV-vis absorption spectroscopy and Raman spectroscopy. The results of X-ray photoelectron spectroscopy reveal that the atomic ration of carbon to oxygen in the RGO can be tuned from1.67to13.7through controlling the reduction time. The electrical measurement shows the conductivity of the RGO to be2.7x104s.m-1, much larger than those previously obtained by chemical reduction through other reducing agents. More importantly, the sheet resistance of the RGO film with20nm thickness can be as low as2kΩ, while a high transparency over70%with a broad spectral range from450nm to1500nm can be retained, demonstrating that the produced thin RGO film can be used as a transparent electrode material in a variety of potential application fields such as optoelectronics, photovoltaics and electrochemistry.
In chapter three, a function nanocomposites of RGO-Fe3O4nanoparticles has been chemically synthesized with tunable RGO/Fe3O4ratio. The adsorption behaviors of a series of dyes using these nanocomposites as the adsorbent are systematically investigated through real-time monitoring of the fingerprint spectral changes of the dyes. The results show that, benefiting both from the surface property of RGO and from the magnetic property of Fe3O4, the nanocomposites possess quite a good adsorption capacity to the dyes, and can be easily and rapidly extracted from water by magnetic attraction. Most importantly, it is found that by simply annealing in moderate conditions, this adsorbent can be easily and efficiently regenerated for reuse with hardly any compromise of the adsorption capacity. Furthermore, the adsorbability of this adsorbent shows satisfactory tolerance against the variations in both pH environment and dye concentration. Even when exposed to a multi dye cocktail, this adsorbent can work well without suppressing the adsorption capacity for each of the dyes, as compared with that measured separately. The RGO-Fe3O4nanocomposites with many excellent abilities can be as a promising candidate for highly-efficient dye pollutant removal.
In chapter four, we, for the first time, reported the successful synthesis of RGO-Pd cluster nanocomposite in water solution. HRTEM/TEM and XRD measurements reveal that the nanocomposites contain amorphous Pd clusters with the size of2nm on the matrix of RGO. Based on the results of a serious of control experiments, we proposed the possible mechanism for the preparation of nanocomposite as following. The Pd2+is first coordinated by NH3effectively to form Pd(NH3)42+, and then the Pd(NH3)42+can adsorb onto the GO surface through opposite charges interaction, whereafter both GO and Pd2+will be reduced to form the RGO-Pd cluster nanocomposite under the irradiation of high pressure mercury lamp. Compared to the RGO-PdNPs, the RGO-Pd cluster nanocomposites holds higher catalytic activity and stability for the oxygen reduction reaction of formic acid under the same conditions, making the RGO-Pd cluster as a good new catalyst for fuel cell.
引文
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