纳米金及金/凹凸棒土复合材料的制备与表征
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摘要
金纳米材料的特殊性能已经被广泛应用于光电子学,生物医学以及催化等领域。尽管目前在金纳米粒子的形貌和尺寸控制生长以及性能研究方面已经取得了巨大进展,但是对于探索环境友好并更具有实用价值的合成方法仍旧是人们关注的热点。本文通过使用不同化学方法合成了粒径以及形状各异的金纳米粒子材料,采用TEM、HRTEM、SEM、XRD、SAED、EDS和UV-vis等手段对所制备的金纳米粒子的形貌、尺寸、晶体结构以及光学性质等进行了表征,并初步探索了各种形状金纳米粒子的生长机理。
本文的研究内容主要包括:
1.通过改变反应中的氯金酸和柠檬酸钠的摩尔比例来调控金纳米粒子的粒径和形状,结果表明,制备的纳米金颗粒呈球形,为面心立方结构;柠檬酸钠作为还原剂不但提高了金颗粒的单分散性和稳定性,还在一定程度上抑制了金纳米粒子的生长,使得其粒径可控,且分布均匀。紫外-可见吸收光谱反映出,随着粒径的增大,纳米金在可见光区域的吸收峰发生红移。
2.利用乳酸作为还原剂制备的金纳米粒子,通过XRD分析产物的衍射峰得出分别对应于金的(111),(200),(220)和(311)晶面,证明了金纳米粒子的晶体结构是面心立方结构。由高分辨率透射图可知由相邻条纹间的面间距为0.233 nm,与面心立方结构金的(111)晶面相对应。实验发现氯金酸和乳酸的摩尔比强烈影响着金纳米粒子的粒径和形状,基于此结果,提出了合成金纳米颗粒的机理。由于金纳米粒子优良的生物相容性以及在乳酸水溶液中的易溶性,通过该方法制备出的金纳米粒子将来在生物和医学上有更多的应用。
3.结果表明,十六烷基三甲基溴化铵(CTAB)、银离子的浓度和溶液的pH值在合成金纳米棒过程中有着重要作用。在十六烷基三甲基溴化铵(CTAB)和硝酸银浓度一定的条件下,研究了溶液pH值对金纳米粒子生长过程的影响,所获得的金纳米粒子形貌和尺寸分布与溶液pH值密切相关。研究结果表明:金纳米棒的尺寸和形貌在很大程度上取决于溶液的pH值。在弱酸性和高浓度的CTAB的条件下,能够合成出高产率的金纳米棒。在合成过程中,CTAB不仅作为表面活性剂,而且作为形成金纳米棒的引导剂。高分辨电镜结果表明,金纳米棒为单晶结构,沿[100]晶向生长,从对照实验的结果可知,得出硝酸银的加入量和溶液的pH值强烈影响金纳米棒的形成,同时对合成的金纳米棒进行了初步的机理探讨。
4.纳米凹凸棒土是一种新型的天然纳米材料,它具有纤维结构,相互交叉形成“乱稻草堆状”网架结构。此外,凹凸棒土是一种结晶的硅酸盐材料,主要包含Si、O、C等元素,凹凸棒土中含有Mg,Al,Fe,Si等元素;对其性质的研究直接关系到它的工业应用与开发前景。在环境温度为25℃时,抗坏血酸加入量为10μL时,纳米金能更好地吸附到凹凸棒土的孔道内。在环境温度为4℃时,抗坏血酸加入量为20μL时,形成的小尺寸的金纳米粒子填充到凹凸棒土的孔道内。
The special properties of gold nanoparticles have been widely used in the fields of optoelectronics, biomedicine and catalysis. Although the remarkable progress has been achieved in the research of shape and size controlled synthesis and physicochemical properties of gold nanoparticles. However, it is still a challenge to find an environment friendly and practical synthesizing the gold nanoparticles. Different sizes and various shapes of gold nanoparticles are synthesized via cheimcal sol-gel method here. The morphology, size, structure and optical properties of the as-prepared gold nanoparticles were characterized systemically by transmission electron microscopy (TEM), high resolution TEM (HRTEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), selected area electron diffraction (SAED), EDS and UV-vis spectroscopy. A growth mechanism of the gold nanoparticles with different shapes was also discussed.
In this thesis, the following subjects are included:
1. The size and shape of gold nanoparticles are modulated by varying the ratios of chloroauric acid and sodium citrate in the reaction medium. The results indicate that the as-prepared gold nanoparticles with spherical structures are face center cubic( FCC). Sodium citrate not only improves monodispersity and stability of gold nanoparticles, but also restrains their crystal growth, which makes the nanoparticles with a narrow size distribution and controllable size. The peak positions of UV-Vis absorption spectra exhibit a blue-shift as the crystal size decreases.
2. A synthesis method of green chemistry of gold nanoparticles using lactic acid as a reducing agent is reported. Crystalline nature of the as-prepared gold nanoparticles in the fcc structure is confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0 ), (2 2 0) and (3 1 1) planes, which are bright circular spots in the SAED and clear lattice fringes in the HRTEM image. It is found that the size and shape of gold nanoparticles are strongly influenced by the molar ratio of HAuCl4 to lactic acid. Based on these results, a potential mechanism of this prepared method of gold nanoparticle is also discussed. It could be found more biological and medical applications of gold nanoparticles based on their biocompatibility and solubility in aqueous solutions of lactic acid in this novel method in future.
3. These result suggest that the pH values of growth solution, CTAB concentration and silver ions concentration play the important role in the process of the as-synthesized gold nanorods. The results showed that the size and morphology of the as-prepared gold nanoparticles were much affected by the solution pH. A synthetic method of high-yield gold nanorods at weak acidic condition and higher cetyltrimethylammonium bromide (CTAB) concentrations was reported. Here, CTAB is not only a stable agent for nanoparticles but also is an inductive agent for forming gold nanorods. The single-crystalline nature of gold nanorods with an oriented growth along the [100] axis direction was confirmed by HRTEM. Based on the controlled experiments, the formation of the gold nanorod are strongly influenced by the concentrations of silver ions and different pH. A possible mechanism for synthesis of gold nanorods was also discussed.
4. Attapulgite is a new type of natural nanomaterials with a fiber structure, formed the intersection "wild straw-like" network structure. Attapulgite is a crystalline silicate materials, mainly containing Si, O, C and some other elements. Moreover, attapulgite contains a considerable content of Mg, Al, Fe, Si elements.It is important to investigate their properties for their applications in industry in furtue. Under condition of 10μL of ascorbic acid as the reduced agent, gold nanoparticles were adsorbed to the on the surface of attapulgite at 25℃. Under condition of 20μL of ascorbic acid as the reduced agent, the gold nanoparticles with small sizes were filled into the channels of attapulgite at 4℃forming nanocomposites.
本文的研究内容主要包括:
1.通过改变反应中的氯金酸和柠檬酸钠的摩尔比例来调控金纳米粒子的粒径和形状,结果表明,制备的纳米金颗粒呈球形,为面心立方结构;柠檬酸钠作为还原剂不但提高了金颗粒的单分散性和稳定性,还在一定程度上抑制了金纳米粒子的生长,使得其粒径可控,且分布均匀。紫外-可见吸收光谱反映出,随着粒径的增大,纳米金在可见光区域的吸收峰发生红移。
2.利用乳酸作为还原剂制备的金纳米粒子,通过XRD分析产物的衍射峰得出分别对应于金的(111),(200),(220)和(311)晶面,证明了金纳米粒子的晶体结构是面心立方结构。由高分辨率透射图可知由相邻条纹间的面间距为0.233 nm,与面心立方结构金的(111)晶面相对应。实验发现氯金酸和乳酸的摩尔比强烈影响着金纳米粒子的粒径和形状,基于此结果,提出了合成金纳米颗粒的机理。由于金纳米粒子优良的生物相容性以及在乳酸水溶液中的易溶性,通过该方法制备出的金纳米粒子将来在生物和医学上有更多的应用。
3.结果表明,十六烷基三甲基溴化铵(CTAB)、银离子的浓度和溶液的pH值在合成金纳米棒过程中有着重要作用。在十六烷基三甲基溴化铵(CTAB)和硝酸银浓度一定的条件下,研究了溶液pH值对金纳米粒子生长过程的影响,所获得的金纳米粒子形貌和尺寸分布与溶液pH值密切相关。研究结果表明:金纳米棒的尺寸和形貌在很大程度上取决于溶液的pH值。在弱酸性和高浓度的CTAB的条件下,能够合成出高产率的金纳米棒。在合成过程中,CTAB不仅作为表面活性剂,而且作为形成金纳米棒的引导剂。高分辨电镜结果表明,金纳米棒为单晶结构,沿[100]晶向生长,从对照实验的结果可知,得出硝酸银的加入量和溶液的pH值强烈影响金纳米棒的形成,同时对合成的金纳米棒进行了初步的机理探讨。
4.纳米凹凸棒土是一种新型的天然纳米材料,它具有纤维结构,相互交叉形成“乱稻草堆状”网架结构。此外,凹凸棒土是一种结晶的硅酸盐材料,主要包含Si、O、C等元素,凹凸棒土中含有Mg,Al,Fe,Si等元素;对其性质的研究直接关系到它的工业应用与开发前景。在环境温度为25℃时,抗坏血酸加入量为10μL时,纳米金能更好地吸附到凹凸棒土的孔道内。在环境温度为4℃时,抗坏血酸加入量为20μL时,形成的小尺寸的金纳米粒子填充到凹凸棒土的孔道内。
The special properties of gold nanoparticles have been widely used in the fields of optoelectronics, biomedicine and catalysis. Although the remarkable progress has been achieved in the research of shape and size controlled synthesis and physicochemical properties of gold nanoparticles. However, it is still a challenge to find an environment friendly and practical synthesizing the gold nanoparticles. Different sizes and various shapes of gold nanoparticles are synthesized via cheimcal sol-gel method here. The morphology, size, structure and optical properties of the as-prepared gold nanoparticles were characterized systemically by transmission electron microscopy (TEM), high resolution TEM (HRTEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), selected area electron diffraction (SAED), EDS and UV-vis spectroscopy. A growth mechanism of the gold nanoparticles with different shapes was also discussed.
In this thesis, the following subjects are included:
1. The size and shape of gold nanoparticles are modulated by varying the ratios of chloroauric acid and sodium citrate in the reaction medium. The results indicate that the as-prepared gold nanoparticles with spherical structures are face center cubic( FCC). Sodium citrate not only improves monodispersity and stability of gold nanoparticles, but also restrains their crystal growth, which makes the nanoparticles with a narrow size distribution and controllable size. The peak positions of UV-Vis absorption spectra exhibit a blue-shift as the crystal size decreases.
2. A synthesis method of green chemistry of gold nanoparticles using lactic acid as a reducing agent is reported. Crystalline nature of the as-prepared gold nanoparticles in the fcc structure is confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0 ), (2 2 0) and (3 1 1) planes, which are bright circular spots in the SAED and clear lattice fringes in the HRTEM image. It is found that the size and shape of gold nanoparticles are strongly influenced by the molar ratio of HAuCl4 to lactic acid. Based on these results, a potential mechanism of this prepared method of gold nanoparticle is also discussed. It could be found more biological and medical applications of gold nanoparticles based on their biocompatibility and solubility in aqueous solutions of lactic acid in this novel method in future.
3. These result suggest that the pH values of growth solution, CTAB concentration and silver ions concentration play the important role in the process of the as-synthesized gold nanorods. The results showed that the size and morphology of the as-prepared gold nanoparticles were much affected by the solution pH. A synthetic method of high-yield gold nanorods at weak acidic condition and higher cetyltrimethylammonium bromide (CTAB) concentrations was reported. Here, CTAB is not only a stable agent for nanoparticles but also is an inductive agent for forming gold nanorods. The single-crystalline nature of gold nanorods with an oriented growth along the [100] axis direction was confirmed by HRTEM. Based on the controlled experiments, the formation of the gold nanorod are strongly influenced by the concentrations of silver ions and different pH. A possible mechanism for synthesis of gold nanorods was also discussed.
4. Attapulgite is a new type of natural nanomaterials with a fiber structure, formed the intersection "wild straw-like" network structure. Attapulgite is a crystalline silicate materials, mainly containing Si, O, C and some other elements. Moreover, attapulgite contains a considerable content of Mg, Al, Fe, Si elements.It is important to investigate their properties for their applications in industry in furtue. Under condition of 10μL of ascorbic acid as the reduced agent, gold nanoparticles were adsorbed to the on the surface of attapulgite at 25℃. Under condition of 20μL of ascorbic acid as the reduced agent, the gold nanoparticles with small sizes were filled into the channels of attapulgite at 4℃forming nanocomposites.
引文
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