金纳米团簇的可控制备及结构研究
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摘要
金纳米团簇具有独特的原子构型、电子结构及新颖的光学、电学和催化性能,在催化、发光材料、探测设备、生物以及制药等领域有广泛的应用,是近几年以来纳米研究领域的一种新型材料体系,吸引着众多科学家对其进行广泛的研究。目前在该领域仍存在的一些亟需解决的问题,如如何制备出可以精确到原子个数的团簇,如何提高单次制备的产率进而提高最终产量,完善明确团簇结构的方法,是否可以调控团簇的电子原子结构以及如何充分了解其结构与性能间的关联等等。针对这些问题,本论文发展了一种简单、方便、易控的湿化学方法来制备不同尺寸以及不同表面活性剂覆盖的金纳米颗粒,利用同步辐射X射线吸收精细结构谱学(XAFS)技术,透射电镜(TEM)方法和紫外-可见(UV-vis)吸收光谱等实验方法研究了这些金纳米颗粒的尺寸、尺寸分布以及电子原子结构等信息,并对化学环境改变引起的金团簇的原子和电子结构的转变开展了深入研究。此外,本论文结合XAFS技术和X射线衍射(XRD)方法研究了Co掺杂导致的BaTiO3结构相变。
本论文主要包括以下内容：
1.不同尺寸金纳米颗粒的制备
发展了一种简单方便的湿化学反应方法制备出了具有高单分散性(0.1-0.2nm)、尺寸可控的金纳米颗粒(0.9-3.3nm)。本方法的要点是利用金前驱AuClPPh3在乙醇溶剂中的有限溶解度,在弱还原剂的还原下实现颗粒的均匀分布；在不同时间加入强表面活性剂硫醇来控制金纳米颗粒的尺寸。原位XAFS技术对制备过程的研究结果表明,前驱在乙醇溶剂中的溶解度约为1.65mmol/L,随着弱还原反应的进行,初始加入的过量(17.86mmol/L)前驱不断自供给,使得溶液中的金原子浓度逐渐增加,并在反应1h以内都维持在一个很高的浓度,有利于得到高单分散的纳米颗粒。
2.不同表面活性剂对金纳米颗粒影响
制备了大小相近(3nm左右)、不同种类表面活性剂(三苯基膦PPh3,聚乙烯吡咯烷酮PVP,十二胺和十二硫醇)覆盖的金纳米颗粒,研究了不同表面活性剂对纳米颗粒的影响。其中硫醇覆盖样品的空间及尺寸分布最为均匀(3.1±0.1nm),而且硫醇也导致Au-S间发生明显的电子转移。X射线吸收谱表明,PPh3对颗粒的作用最弱,PVP对颗粒的作用有所增加,二者都是通过较弱的分子间作用力与Au颗粒发生作用。十二胺和十二硫醇对颗粒的作用进一步增加,它们与颗粒间能形成明显的化学键(Au-N和Au-S键),并且也导致颗粒内和颗粒表面的Au原子排布的一定程度的无序化。
3.金纳米晶体的表面结构
了解颗粒的真实表面结构是深入理解颗粒表面相关性能的前提。利用化学法制备得到硫醇覆盖的金纳米晶体(3-5nm),并且通过溶剂处理,在保证颗粒尺寸形貌不改变的基础下,移除颗粒表面覆盖的硫醇,使颗粒具有基本“裸露”的表面。X射线吸收谱研究表明,对于硫醇覆盖的样品,颗粒表面的Au-Au键具有较强的收缩(约0.10A),但是对于表面“裸露”的纳米颗粒,颗粒表面的键长收缩并不明显。这一反常的现象主要是因为溶剂与裸露Au颗粒之间的作用降低了其结构扭曲。
4.硫醇脱附及其对金纳米团簇结构的影响
发现利用简单的溶剂交换法可以脱附金纳米晶体和金纳米团簇表面的硫醇分子,并且不会引起颗粒尺寸及其分布的变化。UV-vis和XAFS结果表明这种脱附会导致1.1nm大小的金纳米团簇发生从二十面体到体心立方原子堆积结构的转化。深入的分析表明当溶剂环境从乙醇变换为正己烷时,由于正己烷与硫醇分子间的相互作用,引起团簇表面的电子结构发生改变,硫醇分子从颗粒表面迅速脱离。溶液中“裸露”的金团簇通过重新组合和结构重排,形成扭曲的面心立方结构。
5.Co掺杂对BaTiO3结构的影响
利用固相反应法制备了不同浓度Co(0.01-0.20)掺杂的BaTiO3材料,并且发现这种掺杂会导致BaTiO3材料从四方相相变为高温下才存在的六方相。当Co掺杂浓度低于0.03时,BaTiO3材料仍保持四方相,但当掺杂浓度高于0.05时,BaTiO3材料会发生相变。Co离子的掺杂可以导致BaTiO3从室温四方相相变至只在高温下存在的六方相。XAFS结果表明,掺杂后,Co离子会替代BaTiO3中的Ti离子,这可能是导致材料发生相变的主要因素。
Gold nanoclusters with specific electronic and atomic structures possess unique optic, electronic and catalytic properties and have potential application in fields like catalysis, luminescent material, detector, biology and medicine. Recently, gold nanocluster is one of the newest nanomaterials in nanoscience and trigers great interest for fundamental research. However, before the widely use of gold nanoparticles, there are some unsolved problems blocking the development of this field. Some of these problems include:how to synthesize gold clusters with accurate number of gold atoms; how to improve the yield of gold clusters; how to determine the structure of gold clusters and how to tailor the electronic and atomic structure of gold cluster for the specfic purpose. In this dissertation, by variation chemical parameters, gold nanoparticles with different sizes and capped with differernt surfactants were prepared. With the use of X-ray absorption fine structure (XAFS), transmission electron microscope (TEM) and UV-vis technologies, the size, size distribution, electrnoic and atomic structure of gold nanoparticles were investgated. Besides, we also studied the Co-induced phase transition of BaTiO3by a combination of XAFS and X-ray diffraction (XRD) methods. This dissertation includes:
1. The synthesis of gold nanoparticles with different sizes
A "precursor continuous-supply" strategy was developed for controllable synthesis of0.9-3.3nm Au nanoparticles with a narrow size distribution of0.1-0.2nm, using a weak reductant to slow-down the reducing rate of AuClPPh3precursor in ethanol. Time-dependent x-ray absorption and UV-Vis absorption measurements revealed that owing to the joint use of AuClPPh3and ethanol, the remnant AuClPPh3was self-supplied and the precursor concentration was maintained at a level near to its equilibrium solubility (ca1.65mmol/L) in ethanol. Hence the nucleation duration was extended that focused the initial size distribution of the Au clusters. With reaction going on to58minutes, most of AuClPPh3with a nominal Au concentration of17.86mmol/L was converted to ethanol-soluble Au clusters with the size of about1.0nm, resulting in a high-yield synthesis.
2. Gold nanoparticles capped by different surfactants
Gold nanoparticles passivated by different kinds of surfactants such as triphenylphosphine (PPh3), polyvinylpyrrolidone (PVP), dodecanamine (C12H27N) and dodecanethiol (C12H26S) were prepared and the interactions of Au nanoparticles with different surfactants were also studied. TEM images showed the size of all samples was about3nm and the size distribution of gold nanoparticles could be well controlled by dodecanethiol (3.1±0.1nm). The X-ray absorption near edge spectra manifested the electron transfer between Au and S atoms. For PPh3, PVP, dodecanamine and dodecanethiol covered Au nanoparticles, the atomic structure disorder of Au-Au shell gradually increased in order ranging from0.0095to0.0152A. And dodecanamine and dodecanethiol interacted with Au nanoparticles by forming Au-N or Au-S bond.
3. The surface structure of gold nanocrystals
To compare the surface structure of gold nanocrystals, dodecanethiol passivated gold nanocrystals (3and5nm) and "bare" gold nanocrystals (3and5nm) were prepared. Using in situ X-ray absorption fine structure (XAFS), we are able to distinguish the real surface structure information of the monodispersive sphere-shape Au nanocrystals (NCs) dispersed in hexane solution, in which the NCs are free from the influences of surfactant and polar solvent. It is demonstrated that in such a solution environment the surface Au-Au bond lengths of the naked3and5nm Au NCs are very close to the bulk value, contrary to the strong surface contraction for supported, capped or dried Au NCs. Nevertheless, for the same-sized NCs capped by a strong surfactant such as dodecanethiol, a large surface contraction of-0.10A is observed, most likely due to the stress generated by Au-S interactions..
4. Thiol desorption and its effects on the structure of gold nanoclusters
A solvent-exchange method was proposed to remove thiol molecules from the surface of gold nanocrystals and nanoclusters, while keeping the size and size distribution of gold nanoparticles unchanged. However, the electronic and atomic structures of gold nanoparticles experienced a significant change. It is demonstrated that for dodecanethoil-protected icosahedral Au clusters of1.1nm, solvent-exchange of ethanol by hexane leads to quick desorption of the Au-thiolate protecting layers from the surface, as indicated by XAFS. The survived Au cores then undergo a much slower energy-minimization process via recombination and structural rearrangement, resulting in the formation of distorted face-centered-cubic structured clusters. In response to the dramatically changed atomic structure, the electronic structure of the Au clusters is converted from semiconducting to metallic-like characters.
5. Hexagonal BaTi1-xCoxO3phase stabilized by Co dopants
The phase transition from tetragonal to hexagonal of crystalline BaTi1-xCoxO3(0.01≤x≤0.20) powders prepared by solid state reaction was studied by x-ray diffraction and x-ray absorption fine structure. At the low Co doping level of x≤0.03, the structure of the samples is tetragonal, and it is transformed gradually to a hexagonal structure upon increasing Co content to≥0.05. The detailed analysis of Co K-edge XAFS indicated unambiguously that the doped Co ions are substantially incorporated into the BaTiO3host and likely serve as a trigger in leading the structure transition.
本论文主要包括以下内容：
1.不同尺寸金纳米颗粒的制备
发展了一种简单方便的湿化学反应方法制备出了具有高单分散性(0.1-0.2nm)、尺寸可控的金纳米颗粒(0.9-3.3nm)。本方法的要点是利用金前驱AuClPPh3在乙醇溶剂中的有限溶解度,在弱还原剂的还原下实现颗粒的均匀分布；在不同时间加入强表面活性剂硫醇来控制金纳米颗粒的尺寸。原位XAFS技术对制备过程的研究结果表明,前驱在乙醇溶剂中的溶解度约为1.65mmol/L,随着弱还原反应的进行,初始加入的过量(17.86mmol/L)前驱不断自供给,使得溶液中的金原子浓度逐渐增加,并在反应1h以内都维持在一个很高的浓度,有利于得到高单分散的纳米颗粒。
2.不同表面活性剂对金纳米颗粒影响
制备了大小相近(3nm左右)、不同种类表面活性剂(三苯基膦PPh3,聚乙烯吡咯烷酮PVP,十二胺和十二硫醇)覆盖的金纳米颗粒,研究了不同表面活性剂对纳米颗粒的影响。其中硫醇覆盖样品的空间及尺寸分布最为均匀(3.1±0.1nm),而且硫醇也导致Au-S间发生明显的电子转移。X射线吸收谱表明,PPh3对颗粒的作用最弱,PVP对颗粒的作用有所增加,二者都是通过较弱的分子间作用力与Au颗粒发生作用。十二胺和十二硫醇对颗粒的作用进一步增加,它们与颗粒间能形成明显的化学键(Au-N和Au-S键),并且也导致颗粒内和颗粒表面的Au原子排布的一定程度的无序化。
3.金纳米晶体的表面结构
了解颗粒的真实表面结构是深入理解颗粒表面相关性能的前提。利用化学法制备得到硫醇覆盖的金纳米晶体(3-5nm),并且通过溶剂处理,在保证颗粒尺寸形貌不改变的基础下,移除颗粒表面覆盖的硫醇,使颗粒具有基本“裸露”的表面。X射线吸收谱研究表明,对于硫醇覆盖的样品,颗粒表面的Au-Au键具有较强的收缩(约0.10A),但是对于表面“裸露”的纳米颗粒,颗粒表面的键长收缩并不明显。这一反常的现象主要是因为溶剂与裸露Au颗粒之间的作用降低了其结构扭曲。
4.硫醇脱附及其对金纳米团簇结构的影响
发现利用简单的溶剂交换法可以脱附金纳米晶体和金纳米团簇表面的硫醇分子,并且不会引起颗粒尺寸及其分布的变化。UV-vis和XAFS结果表明这种脱附会导致1.1nm大小的金纳米团簇发生从二十面体到体心立方原子堆积结构的转化。深入的分析表明当溶剂环境从乙醇变换为正己烷时,由于正己烷与硫醇分子间的相互作用,引起团簇表面的电子结构发生改变,硫醇分子从颗粒表面迅速脱离。溶液中“裸露”的金团簇通过重新组合和结构重排,形成扭曲的面心立方结构。
5.Co掺杂对BaTiO3结构的影响
利用固相反应法制备了不同浓度Co(0.01-0.20)掺杂的BaTiO3材料,并且发现这种掺杂会导致BaTiO3材料从四方相相变为高温下才存在的六方相。当Co掺杂浓度低于0.03时,BaTiO3材料仍保持四方相,但当掺杂浓度高于0.05时,BaTiO3材料会发生相变。Co离子的掺杂可以导致BaTiO3从室温四方相相变至只在高温下存在的六方相。XAFS结果表明,掺杂后,Co离子会替代BaTiO3中的Ti离子,这可能是导致材料发生相变的主要因素。
Gold nanoclusters with specific electronic and atomic structures possess unique optic, electronic and catalytic properties and have potential application in fields like catalysis, luminescent material, detector, biology and medicine. Recently, gold nanocluster is one of the newest nanomaterials in nanoscience and trigers great interest for fundamental research. However, before the widely use of gold nanoparticles, there are some unsolved problems blocking the development of this field. Some of these problems include:how to synthesize gold clusters with accurate number of gold atoms; how to improve the yield of gold clusters; how to determine the structure of gold clusters and how to tailor the electronic and atomic structure of gold cluster for the specfic purpose. In this dissertation, by variation chemical parameters, gold nanoparticles with different sizes and capped with differernt surfactants were prepared. With the use of X-ray absorption fine structure (XAFS), transmission electron microscope (TEM) and UV-vis technologies, the size, size distribution, electrnoic and atomic structure of gold nanoparticles were investgated. Besides, we also studied the Co-induced phase transition of BaTiO3by a combination of XAFS and X-ray diffraction (XRD) methods. This dissertation includes:
1. The synthesis of gold nanoparticles with different sizes
A "precursor continuous-supply" strategy was developed for controllable synthesis of0.9-3.3nm Au nanoparticles with a narrow size distribution of0.1-0.2nm, using a weak reductant to slow-down the reducing rate of AuClPPh3precursor in ethanol. Time-dependent x-ray absorption and UV-Vis absorption measurements revealed that owing to the joint use of AuClPPh3and ethanol, the remnant AuClPPh3was self-supplied and the precursor concentration was maintained at a level near to its equilibrium solubility (ca1.65mmol/L) in ethanol. Hence the nucleation duration was extended that focused the initial size distribution of the Au clusters. With reaction going on to58minutes, most of AuClPPh3with a nominal Au concentration of17.86mmol/L was converted to ethanol-soluble Au clusters with the size of about1.0nm, resulting in a high-yield synthesis.
2. Gold nanoparticles capped by different surfactants
Gold nanoparticles passivated by different kinds of surfactants such as triphenylphosphine (PPh3), polyvinylpyrrolidone (PVP), dodecanamine (C12H27N) and dodecanethiol (C12H26S) were prepared and the interactions of Au nanoparticles with different surfactants were also studied. TEM images showed the size of all samples was about3nm and the size distribution of gold nanoparticles could be well controlled by dodecanethiol (3.1±0.1nm). The X-ray absorption near edge spectra manifested the electron transfer between Au and S atoms. For PPh3, PVP, dodecanamine and dodecanethiol covered Au nanoparticles, the atomic structure disorder of Au-Au shell gradually increased in order ranging from0.0095to0.0152A. And dodecanamine and dodecanethiol interacted with Au nanoparticles by forming Au-N or Au-S bond.
3. The surface structure of gold nanocrystals
To compare the surface structure of gold nanocrystals, dodecanethiol passivated gold nanocrystals (3and5nm) and "bare" gold nanocrystals (3and5nm) were prepared. Using in situ X-ray absorption fine structure (XAFS), we are able to distinguish the real surface structure information of the monodispersive sphere-shape Au nanocrystals (NCs) dispersed in hexane solution, in which the NCs are free from the influences of surfactant and polar solvent. It is demonstrated that in such a solution environment the surface Au-Au bond lengths of the naked3and5nm Au NCs are very close to the bulk value, contrary to the strong surface contraction for supported, capped or dried Au NCs. Nevertheless, for the same-sized NCs capped by a strong surfactant such as dodecanethiol, a large surface contraction of-0.10A is observed, most likely due to the stress generated by Au-S interactions..
4. Thiol desorption and its effects on the structure of gold nanoclusters
A solvent-exchange method was proposed to remove thiol molecules from the surface of gold nanocrystals and nanoclusters, while keeping the size and size distribution of gold nanoparticles unchanged. However, the electronic and atomic structures of gold nanoparticles experienced a significant change. It is demonstrated that for dodecanethoil-protected icosahedral Au clusters of1.1nm, solvent-exchange of ethanol by hexane leads to quick desorption of the Au-thiolate protecting layers from the surface, as indicated by XAFS. The survived Au cores then undergo a much slower energy-minimization process via recombination and structural rearrangement, resulting in the formation of distorted face-centered-cubic structured clusters. In response to the dramatically changed atomic structure, the electronic structure of the Au clusters is converted from semiconducting to metallic-like characters.
5. Hexagonal BaTi1-xCoxO3phase stabilized by Co dopants
The phase transition from tetragonal to hexagonal of crystalline BaTi1-xCoxO3(0.01≤x≤0.20) powders prepared by solid state reaction was studied by x-ray diffraction and x-ray absorption fine structure. At the low Co doping level of x≤0.03, the structure of the samples is tetragonal, and it is transformed gradually to a hexagonal structure upon increasing Co content to≥0.05. The detailed analysis of Co K-edge XAFS indicated unambiguously that the doped Co ions are substantially incorporated into the BaTiO3host and likely serve as a trigger in leading the structure transition.
引文
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