Fe_3O_4或γ- Fe_2O_3@Au核—壳结构纳米颗粒的制备，表征，及其在乙型肝炎病毒基因诊断上的应用
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摘要
本文用晶种调制的方法在分散良好的磁性氧化铁纳米颗粒表面异质生长金壳层,从而制备了水溶性Fe3O4或γ-Fe2O3@Au核-壳结构纳米颗粒。从透射电镜照片可以看出,这些复合纳米颗粒相互间分散得很好,而且,它们大致可分为直径小于和大于10纳米的两类颗粒。尽管因金的电子密度比氧化铁的要大,透射电镜较难显示复合纳米颗粒的核-壳结构,但能谱显示在大小粒径两类纳米颗粒中Fe和Au都同时存在。高梯度磁分离的结果分析表明,产物纳米颗粒中纯金颗粒的数目与总量相比完全可以忽略不计。这一结果证实了金壳层在大小粒径纳米颗粒表面的形成,同时也表明,对于大粒径纳米颗粒,其主要成分是金;而小粒径纳米颗粒的主要成分则是氧化铁。通过对金壳层较薄的小粒径纳米颗粒的选区电子衍射花样的研究,我们发现,其衍射环在跟磁性氧化铁和纯金纳米颗粒的衍射环不完全吻合的同时,也具有纯金纳米颗粒的面心立方晶体结构特征。进一步的对比分析表明,这些颗粒的较薄金壳层发生了约12%晶格压缩。我们认为,金壳层之所以发生晶格压缩的驱动力就在于异质界面附近的相干应变,它使得壳层上的金原子以比其通常更紧密的方式排列,以适应磁性氧化铁核纳米颗粒的晶格参数。此外,借助于高梯度磁过滤,我们还研究了合成条件对产物纳米颗粒的影响,发现反应时所用磁性氧化铁晶种纳米颗粒的浓度对纯金纳米颗粒的产率有至关重要的作用;而柠檬酸三钠/金离子摩尔比的作用则主要表现在复合纳米颗粒的金壳层平均厚度上。要使纯金纳米颗粒的产率最小化和复合颗粒有一个适当的壳层厚度,我们认为超顺磁性氧化铁纳米颗粒原液的使用量应介于0.7~1.0毫升之间,而柠檬酸三钠/金离子摩尔比最好限38.85~124.16的范围内。最后,我们还用金纳米颗粒和金包磁性氧化铁纳米颗粒制备了乙型肝炎病毒(hepatitis B virus,HBV)的脱氧核糖核酸(deoxynucleic acid, DNA)探针,并做了简易、经济、快捷地检测HBV DNA的有益尝试。
In this thesis, we describe the synthesis of water-soluble Fe3O4 orγ-Fe2O3@Au nanoparticles through a seed-mediated approach, by which gold shells were hetergeneuously grown onto surfaces of magnetic iron oxide nanoparticles. From TEM images, it is found that these composite nanoparticles are dispersed quite well from each other. Furthermore, the product particles can always be assigned into two categories, one is the particles with a diameter less than 10 nanometer; while the other of relatively larger sizes. Though TEM hardly shows the core-shell structure of these particles (due to the higher electronic density of gold as compared to iron oxde), energy dispersive spectroscopy (EDS) verifies the coexistence of Fe and Au in the concerned particles of either the larger or smaller sizes. This is also confirmed convincingly by results of high-gradient magnetic filtration (HGMF), which demonstrates the negligible amount of pure Au nanoparticles among particles of gold characteristic. Therefore, we conclude that the gold shell do form on surface of magnetic iron oxide nanoparticles, and the large-sized particles are largely of gold character, while the smaller ones of mainly iron composition. For small-sized particles with a relatively thinner gold shell, their selected area electron diffraction (SAED) pattern shares the similarity of face-centered cubic structure with the pattern of pure Au nanoparticles on the one hand, and differs somewhat from that of magnetic iron oxide particles on the other hand. Further comparison between these SAED patterns indicates that about 12% lattice compression had occurred on the relatively thinner gold shell, and the driving force for this, we suggest, is the coherency strain, which enables the shell material at the heterostructured interface to adapt the lattice parameters of the core, causing the Au atoms nearby the heterostructured interface pack more tightly than they usually do in pure Au nanoparticles. With the aid of HGMF, we also investigate influence of the synthetic conditions on the product Fe oxide core/Au shell nanoparticles. The seed concentration is found to play a key role on minimizing the fraction of pure Au nanoparticles, while that of citrate to Au3+ mole ratio affects mainly the mean thickness of gold shell of the product composite nanoparticles. To produce magnetic Fe oxide core/Au shell nanoparticles with a minimum fraction of pure Au particles and suitable thickness of gold shell, 0.7~1.0 ml as-synthesized suspension of the seeded superparamagnetic iron oxide nanoparticles (SPION) and a citrate to Au3+ mole ratio within the 38.85 to 124.16 range are suggested. Finally, we describe preparations of DNA probes labeled with pure Au and composite nanoparticles, as well as their applications in easy, cheap, and fast diagnosis of HBV DNA.
In this thesis, we describe the synthesis of water-soluble Fe3O4 orγ-Fe2O3@Au nanoparticles through a seed-mediated approach, by which gold shells were hetergeneuously grown onto surfaces of magnetic iron oxide nanoparticles. From TEM images, it is found that these composite nanoparticles are dispersed quite well from each other. Furthermore, the product particles can always be assigned into two categories, one is the particles with a diameter less than 10 nanometer; while the other of relatively larger sizes. Though TEM hardly shows the core-shell structure of these particles (due to the higher electronic density of gold as compared to iron oxde), energy dispersive spectroscopy (EDS) verifies the coexistence of Fe and Au in the concerned particles of either the larger or smaller sizes. This is also confirmed convincingly by results of high-gradient magnetic filtration (HGMF), which demonstrates the negligible amount of pure Au nanoparticles among particles of gold characteristic. Therefore, we conclude that the gold shell do form on surface of magnetic iron oxide nanoparticles, and the large-sized particles are largely of gold character, while the smaller ones of mainly iron composition. For small-sized particles with a relatively thinner gold shell, their selected area electron diffraction (SAED) pattern shares the similarity of face-centered cubic structure with the pattern of pure Au nanoparticles on the one hand, and differs somewhat from that of magnetic iron oxide particles on the other hand. Further comparison between these SAED patterns indicates that about 12% lattice compression had occurred on the relatively thinner gold shell, and the driving force for this, we suggest, is the coherency strain, which enables the shell material at the heterostructured interface to adapt the lattice parameters of the core, causing the Au atoms nearby the heterostructured interface pack more tightly than they usually do in pure Au nanoparticles. With the aid of HGMF, we also investigate influence of the synthetic conditions on the product Fe oxide core/Au shell nanoparticles. The seed concentration is found to play a key role on minimizing the fraction of pure Au nanoparticles, while that of citrate to Au3+ mole ratio affects mainly the mean thickness of gold shell of the product composite nanoparticles. To produce magnetic Fe oxide core/Au shell nanoparticles with a minimum fraction of pure Au particles and suitable thickness of gold shell, 0.7~1.0 ml as-synthesized suspension of the seeded superparamagnetic iron oxide nanoparticles (SPION) and a citrate to Au3+ mole ratio within the 38.85 to 124.16 range are suggested. Finally, we describe preparations of DNA probes labeled with pure Au and composite nanoparticles, as well as their applications in easy, cheap, and fast diagnosis of HBV DNA.
引文
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