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單分散貴金屬(Au、AuAg合金)納米顆粒的合成及其性能研究

發(fā)布時間:2018-08-29 10:47
【摘要】:貴金屬納米金及合金材料作為一類新型材料,由于其具有特殊的表面等離子體(SPR)性質、良好的生物相容性和優(yōu)良的催化性等性質,被廣泛應用于催化、生物標記、醫(yī)學診斷、精細化工、燃料電池等領域。研究納米金及合金的合成影響因素、生長機理,探索單分散性貴金屬納米金的可控制備以及探索特定材料的性質及應用是非常重要的。本論文研究中,以模板犧牲法、一步合成法、種子合成法等簡單、易操作的方法合成出單分散性好的貴金屬金、金銀合金納米粒子。利用X-射線粉末衍射(XRD)、紫外-可見吸收(UV-vis)、透射電子顯微鏡(TEM)等分析技術對所制備的納米顆粒的單分散性、組成和晶體結構等基本信息進行了表征和分析,初步探索了合金粒子的性能及其催化應用。通過研究不同溶劑反應過程中合成金納米粒子的單分散性,從而探索溶劑的極性、空間結構與合成最終粒子狀態(tài)之間的定性關系,得出納米顆粒的生長規(guī)律,為進一步研究納米粒子的制備提供一定參考。本論文主要包括三方面的工作:(1)以鉆納米粒子為犧牲模板,合成高度單分散的金納米粒子;所制備的金納米粒子用UV-vis、TEM、XRD等進行分析。結果表明,合成的納米粒子的平均粒徑在5.5nm。通過調整鈷納米粒子和四水合氯金酸(HAuCL4·4H2O)的摩爾比,可以調整最后產物的形貌。(2)主要研究了以油胺為還原劑的油相合成納米金體系中,溶劑的極性及其空間結構對納米金生長及單分散性的影響。通過TEM和UV-vis分析手段,得到產物的光學吸收峰和粒徑的形貌、尺寸及分散性等信息,初步表明溶劑的極性及其空間構型的溶劑對金納米粒子合成的影響的規(guī)律。(3)通過種子調節(jié)生長法,以銀納米粒子為種子,調節(jié)銀種子和氯金酸的摩爾比,合成一系列分散性非常好的AuAg合金納米粒子。進一步對合金紫外吸收光譜上SPR峰與合金粒子的組成進行了研究;與此同時,研究了合金納米粒子對4..硝基苯酚(4-NPh)和硼氫化鈉的反應的催化活性。
[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.
【學位授予單位】:西北大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TB383.1

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