单分散贵金属（Au、AuAg合金）纳米颗粒的合成及其性能研究
发布时间：2018-08-29 10:47
【摘要】：贵金属纳米金及合金材料作为一类新型材料,由于其具有特殊的表面等离子体(SPR)性质、良好的生物相容性和优良的催化性等性质,被广泛应用于催化、生物标记、医学诊断、精细化工、燃料电池等领域。研究纳米金及合金的合成影响因素、生长机理,探索单分散性贵金属纳米金的可控制备以及探索特定材料的性质及应用是非常重要的。本论文研究中,以模板牺牲法、一步合成法、种子合成法等简单、易操作的方法合成出单分散性好的贵金属金、金银合金纳米粒子。利用X-射线粉末衍射(XRD)、紫外-可见吸收(UV-vis)、透射电子显微镜(TEM)等分析技术对所制备的纳米颗粒的单分散性、组成和晶体结构等基本信息进行了表征和分析,初步探索了合金粒子的性能及其催化应用。通过研究不同溶剂反应过程中合成金纳米粒子的单分散性,从而探索溶剂的极性、空间结构与合成最终粒子状态之间的定性关系,得出纳米颗粒的生长规律,为进一步研究纳米粒子的制备提供一定参考。本论文主要包括三方面的工作:(1)以钻纳米粒子为牺牲模板,合成高度单分散的金纳米粒子;所制备的金纳米粒子用UV-vis、TEM、XRD等进行分析。结果表明,合成的纳米粒子的平均粒径在5.5nm。通过调整钴纳米粒子和四水合氯金酸(HAuCL4·4H2O)的摩尔比,可以调整最后产物的形貌。(2)主要研究了以油胺为还原剂的油相合成纳米金体系中,溶剂的极性及其空间结构对纳米金生长及单分散性的影响。通过TEM和UV-vis分析手段,得到产物的光学吸收峰和粒径的形貌、尺寸及分散性等信息,初步表明溶剂的极性及其空间构型的溶剂对金纳米粒子合成的影响的规律。(3)通过种子调节生长法,以银纳米粒子为种子,调节银种子和氯金酸的摩尔比,合成一系列分散性非常好的AuAg合金纳米粒子。进一步对合金紫外吸收光谱上SPR峰与合金粒子的组成进行了研究;与此同时,研究了合金纳米粒子对4..硝基苯酚(4-NPh)和硼氢化钠的反应的催化活性。
[Abstract]:As a new kind of materials, noble metal nanocrystalline gold and alloy materials have been widely used in catalysis, biomarker and medical diagnosis because of their special surface plasma (SPR) properties, good biocompatibility and excellent catalytic properties. Fine chemical industry, fuel cell and other fields. It is very important to study the factors affecting the synthesis and growth mechanism of nano-gold and its alloys, to explore the controllable preparation of monodisperse noble metal nanocrystalline gold, and to explore the properties and applications of specific materials. In this paper, gold and gold alloy nanoparticles with good monodispersity were synthesized by template sacrificial method, one-step synthesis method, seed synthesis method and so on. The monodispersity, composition and crystal structure of the prepared nanoparticles were characterized and analyzed by X-ray powder diffraction (XRD),) UV-Vis absorption (UV-vis) and transmission electron microscopy (TEM). The properties of alloy particles and their catalytic applications were preliminarily explored. By studying the monodispersity of gold nanoparticles synthesized in different solvent reactions, the qualitative relationship between the polarity, spatial structure and the state of the final synthesized particles was explored, and the growth law of nanoparticles was obtained. It provides a certain reference for the further study of the preparation of nanoparticles. This thesis mainly includes three aspects: (1) the highly monodisperse gold nanoparticles were synthesized by using diamond nanoparticles as sacrificial template, and the gold nanoparticles were analyzed by UV-vis,TEM,XRD et al. The results show that the average particle size of the synthesized nanoparticles is 5.5 nm. The morphology of the final product can be adjusted by adjusting the molar ratio of cobalt nanoparticles and chloruronic acid tetrahydrate (HAuCL4 4H2O). (2) the oil phase synthesis of gold nanoparticles using oleamine as reductant was studied. Effects of the polarity and spatial structure of solvents on the growth and monodispersity of gold nanoparticles. By means of TEM and UV-vis, the information of optical absorption peak and particle size, size and dispersity of the product were obtained. The effects of solvent polarity and its spatial configuration on the synthesis of gold nanoparticles were preliminarily indicated. (3) the molar ratio of silver seeds to chloruronic acid was regulated by the method of seed growth and silver nanoparticles were used as seeds. A series of AuAg alloy nanoparticles with excellent dispersion were synthesized. The composition of the SPR peak and the alloy particles in the UV absorption spectra of the alloy was further studied, and the alloy nanoparticles were also studied for the composition of the alloy particles. Catalytic activity of nitrophenol (4-NPh) and sodium borohydride.
【学位授予单位】：西北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1
本文编号：2210969
[Abstract]:As a new kind of materials, noble metal nanocrystalline gold and alloy materials have been widely used in catalysis, biomarker and medical diagnosis because of their special surface plasma (SPR) properties, good biocompatibility and excellent catalytic properties. Fine chemical industry, fuel cell and other fields. It is very important to study the factors affecting the synthesis and growth mechanism of nano-gold and its alloys, to explore the controllable preparation of monodisperse noble metal nanocrystalline gold, and to explore the properties and applications of specific materials. In this paper, gold and gold alloy nanoparticles with good monodispersity were synthesized by template sacrificial method, one-step synthesis method, seed synthesis method and so on. The monodispersity, composition and crystal structure of the prepared nanoparticles were characterized and analyzed by X-ray powder diffraction (XRD),) UV-Vis absorption (UV-vis) and transmission electron microscopy (TEM). The properties of alloy particles and their catalytic applications were preliminarily explored. By studying the monodispersity of gold nanoparticles synthesized in different solvent reactions, the qualitative relationship between the polarity, spatial structure and the state of the final synthesized particles was explored, and the growth law of nanoparticles was obtained. It provides a certain reference for the further study of the preparation of nanoparticles. This thesis mainly includes three aspects: (1) the highly monodisperse gold nanoparticles were synthesized by using diamond nanoparticles as sacrificial template, and the gold nanoparticles were analyzed by UV-vis,TEM,XRD et al. The results show that the average particle size of the synthesized nanoparticles is 5.5 nm. The morphology of the final product can be adjusted by adjusting the molar ratio of cobalt nanoparticles and chloruronic acid tetrahydrate (HAuCL4 4H2O). (2) the oil phase synthesis of gold nanoparticles using oleamine as reductant was studied. Effects of the polarity and spatial structure of solvents on the growth and monodispersity of gold nanoparticles. By means of TEM and UV-vis, the information of optical absorption peak and particle size, size and dispersity of the product were obtained. The effects of solvent polarity and its spatial configuration on the synthesis of gold nanoparticles were preliminarily indicated. (3) the molar ratio of silver seeds to chloruronic acid was regulated by the method of seed growth and silver nanoparticles were used as seeds. A series of AuAg alloy nanoparticles with excellent dispersion were synthesized. The composition of the SPR peak and the alloy particles in the UV absorption spectra of the alloy was further studied, and the alloy nanoparticles were also studied for the composition of the alloy particles. Catalytic activity of nitrophenol (4-NPh) and sodium borohydride.
【学位授予单位】：西北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1
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