石墨烯与金属纳米结构相互作用的研究
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摘要
石墨烯由于其新奇的理化性质,自发现之初一直备受关注,从石墨烯本身的力、热、光、电方面的研究,逐渐扩展为其衍生物与各种其他纳米材料复合物的研究。而金属纳米结构展现出与宏观大块物质和小分子以及其他纳米结构都完全不同的特有性质,如果将它与石墨烯结合起来会产生什么样的奇妙性质,又会带来怎样全新的应用,正是本篇论文研究的重点。本文着眼于石墨烯及其衍生物与金属纳米结构的相互作用,以复合物材料制备为基础,在生物传感、表面增强拉曼散射、催化和荧光等多个方面,探讨这种石墨烯与金属纳米结构复合体系的优势及应用前景。通过表征、计算和讨论,本文认为,合理利用石墨烯与金属纳米结构的相互作用,可以使传感更灵敏,拉曼信号更明显,催化更有效或是荧光更可控。这些研究结果有助于人们进一步理解石墨烯与金属纳米结构的相互作用机理,并为它们在多个领域中的应用提供依据。本论文的主要创新点如下：
1.利用无电沉积技术和一步原位还原法,分别将金纳米颗粒复合到CVD生长石墨烯和化学氧化还原石墨烯上。通过电子显微镜、能量散射谱及X光电子能谱的测量手段进行详细表征分析。
2.提出利用CVD石墨烯与金纳米颗粒复合物痕量检测的方法。利用这种方法,β2受体激动剂可以被灵敏、便捷的检测出。这个工作为严格控制p2受体激动剂类药物滥用,提供了检测试验新的思路。
3.提出利用石墨烯与金纳米颗粒复合物作为表面增强拉曼散射(SERS)衬底的方法,对罗丹明6G拉曼信号进行测试结果表明,拉曼信号强度有效增强,并进行增强机制的详细分析。这项研究为有效增强拉曼信号提供了新的方法,也为研究之前不易被独立观测的化学机制提供了可能。
4.研究了石墨烯与金纳米颗粒复合物作为催化鲁米诺-过氧化氢化学发光系统的催化剂的表现。系统论证颗粒尺寸效应和石墨烯辅助作用对系统发光强度的影响,提出最优催化条件,在此条件下,利用该发光系统灵敏检测样品中的过氧化氢和多种有机物。
5.提出金属纳米天线调制石墨烯量子点的方法,设计具有多频表面等离子共振(SPR)波段的银纳米八面体结构。利用该种结构SPR与石墨烯量子点发射与激发波段重合的特性,通过时域有限差分法模拟计算,系统考察了银纳米八面体对分布于周围的石墨烯量子点的荧光调控能力。这项研究在衍射极限以下调控石墨烯量子点荧光提供了理论基础,也为石墨烯量子点应用在生物成像和多频光学探头中提供了新的思路。
Graphene has been a concern since the discovery of the beginning, because of its novelty physicochemical properties. The study of graphene is from its own mechanics, calorifics, optics and electricity at the beginning, and now gradually extended into the study of its derivatives with other nanomaterials composite. The unique nature of metallic nanostructures is completely different from macroscopic bulk matter, small molecules or other nano-structures. If it is combined with graphene will produce what kind of wonderful nature, will bring whatnew applications. These are the answers I hope to find in this thesis. Thethesis focuses on the interaction between graphene and its derivatives with metallic nanostructures. Based on the preparation of composite materials, advantages and prospects of graphene with metallic nanostructures composite systems aresystematically discussed in many aspects, such as biosensing, surface-enhanced Raman scattering, catalysis and fluorescence. By characterization, calculation and discussion, the thesis argues that rational use of the interaction of graphene and metallic nanostructures can make more sensitive sensor, the Raman signal more obvious, catalysis more effective orfluorescence more controllable. These findings will help people further understand the mechanism of interaction of graphene with metallic nanostructures, and provide application basis in many areas. The main innovations of this thesis are as below:
1. In the preparation of graphene and metal nanostructures, using electroless deposition techniques and in situ reduction step, the gold particles are compounded into the CVD growth graphene and chemical redox graphene, respectively. Electron microscopy, energy dispersive spectroscopy and X-ray photoelectron spectroscopy results show that the metal particles can be uniformly dispersed in the graphene sheet or edges.(J. NanoscI. Nanotechno.2014,14,3412; Paten, CN102513533A)
2. In biosensing, in order to be more sensitive and convenient detection of β2agonist, the graphene and gold nanoparticles compositesare used to trace detectβ2agonist. Using this method, β2agonists detection limit is down to10-10M, and the concentration of the analyte can be detected in the linear range:10-6～10-10M. To strictly control the β2agonist class of drugs abuse, this work provides a new testing idea.(Chinanano2013,135; Talanta2013,115,992; Chem. Phys. Lett.2013,574,83;)
3. In the surface-enhanced Raman scattering (SERS), the proposed graphene and gold nanoparticles composites are used as a method of SERS substrate.The Raman signal of Rhodamine6G test results show that the enhancing effect of composite substrate is much better than pure gold nanoparticles substrate. More importantly,by further test and discussion in detail, the composite substrate is a very suitable means for SERS enhancement of chemical mechanisms. These findings would provide a new insight on better understanding of chemical-enhanced Raman mechanism and open up a new way of the graphene-metallic nanoparticle substrate applications.(Chem. Phys. Lett.2013,582,119)
4. In catalysis, the chemiluminescence (CL) performance of luminol is improved using graphene and gold nanoparticle composites as catalyst. The size effect of particle and the assisted enhancement effect of graphene are studied and discussed in detail. Based on the discussion, an optimal, sensitive and stable CL system is proposed. Finally, we utilize the system as a sensor to detect hydrogen peroxide and organic compounds containing amino, hydroxyl, or thiol groups. The CL system might provide a more attractive platform for various analytical devices with CL detection in the field of biosensors, bioassays and immunosensors.(Chinese Phys. B2014,23,048103)
5. In terms of fluorescence modulation, an effective strategy to enhance and modulate the photoluminescence (PL) of graphene quantum dots (GQDs) in the vicinity of a single silver nano-octahedron (SNO) is proposed utilizing three-dimensional finite-difference time-domain calculations. The SNO is designed to act as a multifrequency plasmonic antenna with multiple plasmon resonance modes covering multiple emission peaks of GQDs. The spectral modifications of spontaneous emission are investigated with the variations of the GQD's position and dipole moment orientation relative to the SNO. The PL colour of the GQD can be precisely adjusted between blue and green through the strong interaction with the designed antenna. The multicolour features of GQDs will also facilitate their potential applications as eco-friendly and multifunctional optical probes. The study contributes to a deeper understanding of the PL properties of GQDs near the metallic nanoparticles.(.Phys. Chem. Chem. Phys.2014,16,4504)
1.利用无电沉积技术和一步原位还原法,分别将金纳米颗粒复合到CVD生长石墨烯和化学氧化还原石墨烯上。通过电子显微镜、能量散射谱及X光电子能谱的测量手段进行详细表征分析。
2.提出利用CVD石墨烯与金纳米颗粒复合物痕量检测的方法。利用这种方法,β2受体激动剂可以被灵敏、便捷的检测出。这个工作为严格控制p2受体激动剂类药物滥用,提供了检测试验新的思路。
3.提出利用石墨烯与金纳米颗粒复合物作为表面增强拉曼散射(SERS)衬底的方法,对罗丹明6G拉曼信号进行测试结果表明,拉曼信号强度有效增强,并进行增强机制的详细分析。这项研究为有效增强拉曼信号提供了新的方法,也为研究之前不易被独立观测的化学机制提供了可能。
4.研究了石墨烯与金纳米颗粒复合物作为催化鲁米诺-过氧化氢化学发光系统的催化剂的表现。系统论证颗粒尺寸效应和石墨烯辅助作用对系统发光强度的影响,提出最优催化条件,在此条件下,利用该发光系统灵敏检测样品中的过氧化氢和多种有机物。
5.提出金属纳米天线调制石墨烯量子点的方法,设计具有多频表面等离子共振(SPR)波段的银纳米八面体结构。利用该种结构SPR与石墨烯量子点发射与激发波段重合的特性,通过时域有限差分法模拟计算,系统考察了银纳米八面体对分布于周围的石墨烯量子点的荧光调控能力。这项研究在衍射极限以下调控石墨烯量子点荧光提供了理论基础,也为石墨烯量子点应用在生物成像和多频光学探头中提供了新的思路。
Graphene has been a concern since the discovery of the beginning, because of its novelty physicochemical properties. The study of graphene is from its own mechanics, calorifics, optics and electricity at the beginning, and now gradually extended into the study of its derivatives with other nanomaterials composite. The unique nature of metallic nanostructures is completely different from macroscopic bulk matter, small molecules or other nano-structures. If it is combined with graphene will produce what kind of wonderful nature, will bring whatnew applications. These are the answers I hope to find in this thesis. Thethesis focuses on the interaction between graphene and its derivatives with metallic nanostructures. Based on the preparation of composite materials, advantages and prospects of graphene with metallic nanostructures composite systems aresystematically discussed in many aspects, such as biosensing, surface-enhanced Raman scattering, catalysis and fluorescence. By characterization, calculation and discussion, the thesis argues that rational use of the interaction of graphene and metallic nanostructures can make more sensitive sensor, the Raman signal more obvious, catalysis more effective orfluorescence more controllable. These findings will help people further understand the mechanism of interaction of graphene with metallic nanostructures, and provide application basis in many areas. The main innovations of this thesis are as below:
1. In the preparation of graphene and metal nanostructures, using electroless deposition techniques and in situ reduction step, the gold particles are compounded into the CVD growth graphene and chemical redox graphene, respectively. Electron microscopy, energy dispersive spectroscopy and X-ray photoelectron spectroscopy results show that the metal particles can be uniformly dispersed in the graphene sheet or edges.(J. NanoscI. Nanotechno.2014,14,3412; Paten, CN102513533A)
2. In biosensing, in order to be more sensitive and convenient detection of β2agonist, the graphene and gold nanoparticles compositesare used to trace detectβ2agonist. Using this method, β2agonists detection limit is down to10-10M, and the concentration of the analyte can be detected in the linear range:10-6～10-10M. To strictly control the β2agonist class of drugs abuse, this work provides a new testing idea.(Chinanano2013,135; Talanta2013,115,992; Chem. Phys. Lett.2013,574,83;)
3. In the surface-enhanced Raman scattering (SERS), the proposed graphene and gold nanoparticles composites are used as a method of SERS substrate.The Raman signal of Rhodamine6G test results show that the enhancing effect of composite substrate is much better than pure gold nanoparticles substrate. More importantly,by further test and discussion in detail, the composite substrate is a very suitable means for SERS enhancement of chemical mechanisms. These findings would provide a new insight on better understanding of chemical-enhanced Raman mechanism and open up a new way of the graphene-metallic nanoparticle substrate applications.(Chem. Phys. Lett.2013,582,119)
4. In catalysis, the chemiluminescence (CL) performance of luminol is improved using graphene and gold nanoparticle composites as catalyst. The size effect of particle and the assisted enhancement effect of graphene are studied and discussed in detail. Based on the discussion, an optimal, sensitive and stable CL system is proposed. Finally, we utilize the system as a sensor to detect hydrogen peroxide and organic compounds containing amino, hydroxyl, or thiol groups. The CL system might provide a more attractive platform for various analytical devices with CL detection in the field of biosensors, bioassays and immunosensors.(Chinese Phys. B2014,23,048103)
5. In terms of fluorescence modulation, an effective strategy to enhance and modulate the photoluminescence (PL) of graphene quantum dots (GQDs) in the vicinity of a single silver nano-octahedron (SNO) is proposed utilizing three-dimensional finite-difference time-domain calculations. The SNO is designed to act as a multifrequency plasmonic antenna with multiple plasmon resonance modes covering multiple emission peaks of GQDs. The spectral modifications of spontaneous emission are investigated with the variations of the GQD's position and dipole moment orientation relative to the SNO. The PL colour of the GQD can be precisely adjusted between blue and green through the strong interaction with the designed antenna. The multicolour features of GQDs will also facilitate their potential applications as eco-friendly and multifunctional optical probes. The study contributes to a deeper understanding of the PL properties of GQDs near the metallic nanoparticles.(.Phys. Chem. Chem. Phys.2014,16,4504)
引文
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