金、银纳米结构的制备与光学性质研究
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摘要
现代技术的发展与变革在很大程度上依赖于现有材料的改进及新材料的产生。在纳米材料的研究热潮中,贵金属(尤其是Au和Ag)纳米材料因其独特的光、电、催化等特性及其在新能源材料、光电子学、信息存储、生物医疗及表面增强效应等领域的应用而受到众多研究领域的广泛关注。研究表明：金属纳米材料的性能与纳米粒子的尺寸和形貌密切相关。因此对纳米粒子实现可控的生长,并实现按照人的意愿设计合成功能材料具有重要的意义。虽然纳米材料的制备方法日益多样化,但在纳米材料的可控制备方面所取得的成就仍非常有限,因而得到科研工作者越来越多的关注。基于目前贵金属纳米粒子的国内外研究现状,本论文选取金、银纳米粒子作为研究对象,利用简单可行的化学液相法制备了多种形貌可控的金、银纳米结构,并得到了一些新颖的纳米形貌。利用场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)、高分辨透射电镜(HRTEM),X射线衍射仪(XRD)和紫外-可见光光谱仪(UV-Visble)对所得的金、银纳米粒子的结构、形貌和光谱进行表征,并探索了化学反应机理及金、银纳米粒子的生长规律。
本论文的主要结果如下：
1.通过改进PVP (K30, MW=44,000)辅助的多羟基方法,简单快速的一步制备了高产量、形貌完美的银纳米立方体,且立方体的尺寸均一(约230纳米)。研究了温度、PVP/AgNO3的摩尔比对银纳米结构的形貌影响,实验发现温度为150℃、摩尔比为1是合成银纳米立方体的最佳实验参数。随着银纳米立方体尺寸的增加,其表面等离激元共振(SPR)表现明显的红移。从晶体生长的热力学控制和动力学控制两个方面简单讨论了银纳米立方体的生长机制。
2.利用多羟基方法,探讨不同聚合度(链长)的PVP对合成Ag的纳米线的影响。实验发现：用长链的PVP (K90, MW=800,000))可获得产量高、均一性好、长径比较大的银纳米线。研究了银纳米线的光学性质以及生长机制。在反应初期阶段,Ag‘离子与PVP链的极性基团的化学吸附可以促进银纳米线的生长。
3.在改进的多羟基过程中,通过引进短链的PVP(K25, MW=38,000),合成了银纳米线和纳米颗粒的混合物,并研究了样品的表面增强拉曼散射性质。实验发现其拉曼增强因子高于其单一的银纳米线和银纳米颗粒,这种增强效应可能是纳米线与颗粒的耦合效应的结果。通过观察银纳米结构在生长过程中形貌的演变,发现了一个新颖的银纳米线的横向生长过程,提出了银纳米线可能的横向生长机制。TEM结果表明：银颗粒按照纳米线的轴向聚集而促成了银纳米线的横向生长。
4.利用多羟基方法制备尺寸可控的金纳米片(厚度为数十纳米,尺寸在微米量级)。常规方法合成纳米片的形貌以六边形,三角形及截角三角形为主。通过改变温度及PVP/HAuCl4的摩尔比,探讨了金纳米片的最佳生长条件；通过溶剂热的方法,在密封的环境中制备了大尺寸的金纳米片(-50gm)。研究了金纳米片的微观结构和光学性质。
5.在室温条件下,以胶体状态的PVP/HAuCl4为研究对象,在晶体生长的初期阶段,通过对温度进行适当调节,合成了具有新颖形貌的金纳米片(星形、盾形,截角星形等)。研究了PVP聚合度对结果的影响,阐述了新型金纳米片可能的生长过程,其中金的(111)晶面将可能沿着<110>,<211>以及其它高指数方向生长。
The evolution and revolution of all modern technologies strongly depend on the improvement of existing materials and the development of new materials. In the hot research topic of nanomaterials, noble metal (especially for gold and silver) nanostructures have attracted particular attention because of their unique optical, electric, catalytic properties and the promising applications in the fields of new energy materials, optoelectronics, information storage, biomedicine and surface-enhanced Raman scattering. Recent investigations demonstrate that their properties are strongly depended on the size and shape of metal nanoparticles. Therefore, it is important to get the shape-controlled noble metal nanoparticles and design the functional materials. Although there have been a lot of reports on the synthesis of nanomaterials, the shape-controllable synthesis is still a challenge for materials and chemistry researchers. Based on the development of noble metal nanoparticles in the world, this dissertation presents a facile chemical solution method to prepare silver and gold nanoparticles with various morphologies and some nanostructures with novel shapes. Structures, morphology and spectra characterization were carried out by field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electronmicroscopy (HRTEM), X-ray diffraction (XRD) and UV-visible spectrometer (UV-Visble). The chemical reaction and possible growth mechanism were also proposed. The main results of this work are listed as follows:
1. Silver nanocubes with perfect shape were prepared by a simple poly(vinyl pyrrolidone, K30, MW=44,000)-directed polyol synthesis process. Ag nanocubes with an average edge length of230nm were obtained successfully with sharp edges and corners under a precise synthesis condition of R=1and T=150℃. The effects of poly(vinylpyrrolidone)/AgNO3ratio R and reaction temperature T on the morphology and size of the products were investigated. The optical properties of Ag nanocubes show an attractive plasma resonance red-shift with size in a wide spectra region. The growth mechanism of the Ag nanocubes is proposed to be thermodynamically and kinetically controlled.
2. Polyvinyl pyrrolidone (PVP) with different molecular weights was used as capping agent to synthesize silver nanowires through a polyol process. The results indicated that the yields and aspect ratios of silver nanowires were controlled by the chain length of PVP and increased with increasing the molecular weight (MW) of PVP. When the long-chain PVP-K90(MW=800,000) was used, the product was uniform in size and was dominated by nanowires with high aspect ratios. The growth mechanism and optical properties of the nanowires were studied. It is proposed that the chemical adsorption of Ag+on the PVP chains at the initial stage promotes the growth of Ag nanowires.
3. A mixture of Ag nanowires and nanoparticles was obtained by an improved polyol process with the usage of PVP-K25(MW=38,000). Results of Surface-enhanced Raman scattering indicated that the enhancement factor of the wires/particles mixture is larger than that of Ag nanowires and nanoparticles of the mixture. This enhancement should ascribe to the coupling effect of nanowires and nanoparticles. A novel vertical growth process of silver nanowires was revealed by tracing the morphology evolution of Ag nanostructures, in which Ag nanoparticles undergo an important dissolution-recrystallization process and act as fuel for the lateral growth of nanowires. A plausible novel growth mechanism for the silver nanowires was proposed, in which the collection of Ag nanoparticles along the same direction leading to the vertical growth process of Ag nanowires.
4. Gold nanoplates (tens of nanometers in thickness and micrometers in size) have been mass-synthesized through a polyol process. In general methods, most Au nanoplates are regular shapes of triangle and hexagon. The suitable growth conditions for gold nanoplates was studied by changing temperatures and the molar ratios of PVP/HAuCl4. Large sized gold nanoplates with size of～50um were fabricated by a solvent-thermal method.
5. Au nanoplates with novel shapes, involving star-like and shield-like and other novel polygonal are found with introduction of obvious temperature variation in the early crystal growth stage. Structural studies demonstrate that the obtained Au nanoplates are single-crystalline with(111) planes as two growth of (111) plane along <110>,<211> and other high-index directions.
本论文的主要结果如下：
1.通过改进PVP (K30, MW=44,000)辅助的多羟基方法,简单快速的一步制备了高产量、形貌完美的银纳米立方体,且立方体的尺寸均一(约230纳米)。研究了温度、PVP/AgNO3的摩尔比对银纳米结构的形貌影响,实验发现温度为150℃、摩尔比为1是合成银纳米立方体的最佳实验参数。随着银纳米立方体尺寸的增加,其表面等离激元共振(SPR)表现明显的红移。从晶体生长的热力学控制和动力学控制两个方面简单讨论了银纳米立方体的生长机制。
2.利用多羟基方法,探讨不同聚合度(链长)的PVP对合成Ag的纳米线的影响。实验发现：用长链的PVP (K90, MW=800,000))可获得产量高、均一性好、长径比较大的银纳米线。研究了银纳米线的光学性质以及生长机制。在反应初期阶段,Ag‘离子与PVP链的极性基团的化学吸附可以促进银纳米线的生长。
3.在改进的多羟基过程中,通过引进短链的PVP(K25, MW=38,000),合成了银纳米线和纳米颗粒的混合物,并研究了样品的表面增强拉曼散射性质。实验发现其拉曼增强因子高于其单一的银纳米线和银纳米颗粒,这种增强效应可能是纳米线与颗粒的耦合效应的结果。通过观察银纳米结构在生长过程中形貌的演变,发现了一个新颖的银纳米线的横向生长过程,提出了银纳米线可能的横向生长机制。TEM结果表明：银颗粒按照纳米线的轴向聚集而促成了银纳米线的横向生长。
4.利用多羟基方法制备尺寸可控的金纳米片(厚度为数十纳米,尺寸在微米量级)。常规方法合成纳米片的形貌以六边形,三角形及截角三角形为主。通过改变温度及PVP/HAuCl4的摩尔比,探讨了金纳米片的最佳生长条件；通过溶剂热的方法,在密封的环境中制备了大尺寸的金纳米片(-50gm)。研究了金纳米片的微观结构和光学性质。
5.在室温条件下,以胶体状态的PVP/HAuCl4为研究对象,在晶体生长的初期阶段,通过对温度进行适当调节,合成了具有新颖形貌的金纳米片(星形、盾形,截角星形等)。研究了PVP聚合度对结果的影响,阐述了新型金纳米片可能的生长过程,其中金的(111)晶面将可能沿着<110>,<211>以及其它高指数方向生长。
The evolution and revolution of all modern technologies strongly depend on the improvement of existing materials and the development of new materials. In the hot research topic of nanomaterials, noble metal (especially for gold and silver) nanostructures have attracted particular attention because of their unique optical, electric, catalytic properties and the promising applications in the fields of new energy materials, optoelectronics, information storage, biomedicine and surface-enhanced Raman scattering. Recent investigations demonstrate that their properties are strongly depended on the size and shape of metal nanoparticles. Therefore, it is important to get the shape-controlled noble metal nanoparticles and design the functional materials. Although there have been a lot of reports on the synthesis of nanomaterials, the shape-controllable synthesis is still a challenge for materials and chemistry researchers. Based on the development of noble metal nanoparticles in the world, this dissertation presents a facile chemical solution method to prepare silver and gold nanoparticles with various morphologies and some nanostructures with novel shapes. Structures, morphology and spectra characterization were carried out by field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electronmicroscopy (HRTEM), X-ray diffraction (XRD) and UV-visible spectrometer (UV-Visble). The chemical reaction and possible growth mechanism were also proposed. The main results of this work are listed as follows:
1. Silver nanocubes with perfect shape were prepared by a simple poly(vinyl pyrrolidone, K30, MW=44,000)-directed polyol synthesis process. Ag nanocubes with an average edge length of230nm were obtained successfully with sharp edges and corners under a precise synthesis condition of R=1and T=150℃. The effects of poly(vinylpyrrolidone)/AgNO3ratio R and reaction temperature T on the morphology and size of the products were investigated. The optical properties of Ag nanocubes show an attractive plasma resonance red-shift with size in a wide spectra region. The growth mechanism of the Ag nanocubes is proposed to be thermodynamically and kinetically controlled.
2. Polyvinyl pyrrolidone (PVP) with different molecular weights was used as capping agent to synthesize silver nanowires through a polyol process. The results indicated that the yields and aspect ratios of silver nanowires were controlled by the chain length of PVP and increased with increasing the molecular weight (MW) of PVP. When the long-chain PVP-K90(MW=800,000) was used, the product was uniform in size and was dominated by nanowires with high aspect ratios. The growth mechanism and optical properties of the nanowires were studied. It is proposed that the chemical adsorption of Ag+on the PVP chains at the initial stage promotes the growth of Ag nanowires.
3. A mixture of Ag nanowires and nanoparticles was obtained by an improved polyol process with the usage of PVP-K25(MW=38,000). Results of Surface-enhanced Raman scattering indicated that the enhancement factor of the wires/particles mixture is larger than that of Ag nanowires and nanoparticles of the mixture. This enhancement should ascribe to the coupling effect of nanowires and nanoparticles. A novel vertical growth process of silver nanowires was revealed by tracing the morphology evolution of Ag nanostructures, in which Ag nanoparticles undergo an important dissolution-recrystallization process and act as fuel for the lateral growth of nanowires. A plausible novel growth mechanism for the silver nanowires was proposed, in which the collection of Ag nanoparticles along the same direction leading to the vertical growth process of Ag nanowires.
4. Gold nanoplates (tens of nanometers in thickness and micrometers in size) have been mass-synthesized through a polyol process. In general methods, most Au nanoplates are regular shapes of triangle and hexagon. The suitable growth conditions for gold nanoplates was studied by changing temperatures and the molar ratios of PVP/HAuCl4. Large sized gold nanoplates with size of～50um were fabricated by a solvent-thermal method.
5. Au nanoplates with novel shapes, involving star-like and shield-like and other novel polygonal are found with introduction of obvious temperature variation in the early crystal growth stage. Structural studies demonstrate that the obtained Au nanoplates are single-crystalline with(111) planes as two growth of (111) plane along <110>,<211> and other high-index directions.
引文
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