摘要
金原子外层电子之间的相互作用非常紧密，电子不容易被氧化剂夺取，使得金元素化学性质非常稳定并以单质状态散布于矿物质中。Au元素在元素周期表中的位置，决定了它具有很多特殊的性质。十九世纪，Michael Faraday首先发现Au胶体粒子与金黄色的Au块材不同，是一种红色溶液，而且大小不同颜色会发生变化。随着纳米技术的发展，Au纳米结构特殊的表面等离子共振（SPR）、表面增强拉曼散射（SERS）、电学以及催化等性质被揭示，使它在纳米电子学、传感器、生物医药、载药、生物成像、光热治疗、催化、分析、导电和传热等众多领域已经展现出其独特的潜在应用价值，成为学术界广泛研究的热点。Au纳米结构的性能与纳米粒子的组成、尺寸及形貌有着密切的联系，然而，制备超单分散的Au纳米结构的合成条件大都非常苛刻，很难控制；而制备Au复合纳米结构的方法有限且很难控制纳米结构的组成和形貌。因此，组成结构可控的单分散Au纳米结构的制备成为现阶段研究的趋势。本文主要介绍了利用有机密度梯度速率离心分离的方法获得单分散的Au纳米结构以及利用化学转化控制Au复合纳米结构，具体的研究工作及研究结果包括：
1. Au纳米结构的有机密度梯度速率离心分离
将一种纯液相、无破坏、适用性广的分离手段——密度梯度速率离心分离法拓展到有机相，发展了有机密度梯度速率离心分离法。利用此法将未经预处理的包含表面活性剂分子的原始Au胶体粒子进行了分离和纯化，获得了多种尺寸的超单分散Au纳米颗粒。对直径<2nm的超细Au纳米线/Au纳米颗粒混合物进行了分离，由于Au纳米线大的长径比，使它在运动中的摩擦力增大，而被留在梯度液的顶部，从而使纳米线与纳米颗粒得到了分离。分离后的单分散Au纳米粒子可以直接在乙醇和环己烷的界面处组装，得到六边形密堆积的超晶格结构。同时，我们将此有机密度梯度速率分离体系拓展到了Ag纳米粒子、CdSe和CdS半导体纳米粒子，以及Fe3O4等磁性纳米粒子的分离，也获得了成功。特别是在CdSe半导体的分离中，分离将原始较为单分散的CdSe胶体粒子的荧光半峰宽从~100nm降低到50nm。另一方面，将高分子PS（聚苯乙烯）引入梯度介质中，增加了梯度液的粘度，使分离效果提高。最后，以CdSe纳米粒子作为探针分子，考察了梯度液的坡度和粘度对分离效果的影响。
2. Au纳米结构的转化
根据李亚栋等报道的方法，合成出Au纳米复合结构Au-Ni异质结构。由于很多文献报道，卤素离子在贵金属纳米结构的合成中对形貌有很大影响，我们将DDAB（双十二烷基二甲基溴化铵）引入到Au纳米结构的化学转化中，以溶解有DDAB或OA(油胺)的HAuCl_4·4H_2O溶液作为前驱体，对Au-Ni异质结构进行化学转化。由于不同配体的调控作用不同，使得这两种前驱体与Au-Ni异质结构发生着两种截然不同的反应。在含有OA的前驱体中，随着前驱体量的增大，Au“头”逐渐变大，Ni“尾”逐渐减小。但在含有DDAB的前驱体中，我们发现随着前驱体量的增加，Au“头”首先逐渐消失，后又出现，然后再溶解，最终得到空心的NiO纳米晶。通过HRTEM、UV-vis、EDS等的表征结果和一系列的对比实验，我们提出了反应的机理：在Au-Ni异质结构的外部有一薄层的NiO壳，NiO在含有OA的前驱体中先被溶解，然后Ni“尾”被Au~(3+)氧化而变小，Au通过油胺的还原和Ni的置换而长大。在含有DDAB的前驱体中，Au~(3+)和Au~0在DDAB存在的情况下可以反应生成AuBr，而且由于NiO的保护作用，使得此体系中Ni被保护，Au首先被溶解，Au溶解完之后在Au和Ni的界面处开始Ni与Au~(3+)的置换反应，此时Ni开始溶解并伴随着新的Au纳米晶的生成；当溶解有DDAB的HAuCl4·4H2O前驱体的量继续增大，新的Au也被溶解，留下NiO的空心结构。利用这种以异质结构为模板，通过配体的调控进行低对称Au复合纳米结构的选择性化学转化，可以拓展到更多的纳米材料和配体中，为更多的非对称功能复合纳米结构的调控提供了新的方法。
Close interaction between the outer electrons makes gold chemicallystable and hard to be oxidized. Therefore, gold always exits as elementalstate in the minerals. The position of gold in the periodic table indicatesits special properties. In the1800s, Michael Faraday found that a solutionof nanometer-sized gold particles was red in color, unlike the yellowcolor of bulk gold, and that varying the size of the particle s could changethe color of the colloid. With the development of nanotechnology, manyspecial properties of gold nanostructures such as surface plasmonresonance (SPR), surface-enhanced Raman scattering (SERS), electricaland catalytic properties have been demonstrated, which make goldnanostructures potential candidates in many areas such as nanoelectronics,sensors, bio-medicine, drug delivery, biological imaging, photothermaltherapy, catalysis, analysis, conductivity and heat transfer, etc. Recently,research on gold nanostructures has been a hotspot. The properties of gold nanostructures closely related to their composition, size andmorphology, however, fabrication of monodisperse gold nanostructurealways need strict synthetic conditions and synthesis of goldnanocomposite lacks accurate control of the composition. Thus, researchon the fabrication of monodisperse gold nanoparticles with controlledcomposition has been a research direction. In this thesis, we demonstratea density gradient rate separation method to obtain monodisperse goldnanoparticles along with a chemical transformation of goldnanocomposite. Details are illustrated as follows:
1. Density gradient rete separation of gold nanostructures inorganic media
We expanded a pure liquid phase, no damage and wide applicableseparation method, density gradient rete separation, into organic media.Through this method, non-pretreatment gold nanoparticles with surfactantmolecules attached on the surface could be isolated by size and severalmonodisperse gold nanoparticles with certain diameters could be obtained.This method could also be applied to ultra-fine goldnanowire/nanoparticle system. Large aspect ratio of ultra-fine nanowireincreased its friction and made it stayed on the top of the gradient, whilethe nanoparticles fell down and thus separation achieved. Themonodisperse gold nanoparticles obtained after separation could assembleinto superlattice at the interface of ethanol and cyclohexane. Furthermore, the success on separation of gold nanostructures could be expaneded tolots of other nanostructures like noble metals (Ag), semiconductors (CdSe,CdS) and magnetic nanoparticles (Fe_3O_4, Au/Co, Au/Ni) and so on.Specially, in the separation CdSe nanoparticles, we used relativelymonodisperse nanoparticles, after separation, the half peak width of theoriginal “monodisperse” samples in the fluorescence was successfullyreduced from100nm to50nm, which confirmed the efficiency of densitygradient rete separation. We have also introduced polymers into thegradients to increase the viscosity; results indicated that viscosity increasecould enhance the separation efficiency. Finally, CdSe nanoparticles wereused as probe molecule to study the influence of viscosity and slope ofthe gradient.
2. Transformation of gold nanostructures
Au–Ni spindly nanostructures were synthesized using the methodreported by Wang and Li. Many reports have shown that halogen ionsplay important roles in synthesis and conversion of noble metalnanoparticles by interfering with the reaction process. Here we introducedDDAB and OA into the Au-Ni system to study the chemicaltransformation of Au-Ni heteronanostructures. Different ligands results indifferent reactions. When increasing quantities of OA-containingHAuCl4·4H2O solutions were gradually added to solutions of the Au–Ninanoparticles, the Au tips grew larger while the Ni tails gradually dissolved. However, when OA was replaced by DDAB, the results werecompletely different. As the amount of DDAB-containing HAuCl4·4H2Osolution was increased, the Au tips first shrank and then vanished leavinga bowl-like structure. Subsequently the Ni tails dissolved leaving asemi-filled sphere within which new Au cores were generated. Finally,the newly generated Au cores mostly disappeared again, leaving hollownanospheres. HRTEM, UV-Vis spectroscope, EDS and a series of controlexperiments helps us to propose a mechanism of the two differenttransformation routes: we propose that the rapid reaction between Au–Niand the DDAB-containing HAuCl_4·4H_2O solution leads to the initialdissolution of the Au tips, while the NiO layer prevents any redoxreaction between Au~(3+)and Ni, resulting in selective etching of the Au.However, such etching of Au at the “neck” sections of the original Au–Niheterostructures eventually exposes fresh Ni metal not protected by alayer of NiO, and when larger quantities of DDAB-containingHAuCl4·4H2O solution were added, etching of the exposed Ni metal leadsto a “bowl-like” Ni tail with a NiO layer. The new Au cores generatedfrom the galvanic replacement reaction between Ni metal and Au~(3+)aremostly located at the openings/cores of the “bowls”. Eventually the Nitail dissolves completely leaving Au cores inside or attached to the NiOshell. Finally, the redox reaction between the Au cores and theDDAB-containing HAuCl_4·4H_2O solution restarts until most of the regenerated Au cores redissolved again. The ability to tailor thecompositions and structures of heterostructures with low symmetryshould benefit finely manipulation on their properties and lead to newbuilding blocks for the construction of new functional nanomaterials.
引文
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