稀土化合物纳米材料的液相控制合成、形成机理及性能研究
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摘要
稀土化合物纳米材料具有优越的光学、电学、磁学性质,而且在激光施主材料、光学纤维、湿度传感器、发光材料、磁材料、催化材料、抗菌材料等方面具有广泛的应用前景,因此控制合成稀土化合物纳米材料,探索其性质与尺寸、形貌的依赖特性,开发稀土化合物新的应用领域,已成为材料研究的热点之一。另外,我国的稀土资源储量居世界第一位,利用这样的资源优势,开发研究新型的稀土化合物纳米材料,推动其在各产业领域中的应用,将具有十分重要的经济价值和社会价值。本论文中,我们通过室温水相、水热法、溶剂热等液相技术合成一系列的稀土化合物纳米材料,主要的工作包括以下几方面:
(1)在无表面活性剂或模板剂的条件下,室温水相反应体系成功地合成出系列轻稀土磷酸盐LnPO4·nH2O(Ln=La-Gd)(n=0～1)和氢氧化物Ln(OH)3(Ln=La-Gd)一维纳米材料。一维纳米材料的形成主要是由六方晶相结构的轻稀土磷酸盐和氢氧化物的各向异性所决定的,它的长径比还与反应体系的pH值和反应时间有关。并研究不同长度Eu3+:LaPO4纳米线和Eu(OH)3纳米棒的室温光学性质,我们发现纳米线的发光强度与结晶度和形貌有关。研究表明:轻稀土化合物具有类似的化学性质和形貌,但也有展示独特的个性(如在同样的实验条件,我们合成出重稀土单斜相YPO4·2H2O纳米线的合成)。
(2)以有机络合剂辅助合成的水热体系,通过简单的稀土硝酸化合物与原钒酸钠反应合成出多种多级组装结构的重稀土钒酸盐化合物(YVO4、DyVO4、ErVO4)纳米材料,如纳米柿球、纳米立方体组装结构和纳米粒子等,并对纳米柿球的组装结构形成机理进行了较为系统的研究。研究表明:反应时间、稀土离子与络合剂摩尔比、络合剂的种类以及稀土离子的半径对重稀土钒酸盐的组装结构均具有重要的影响;纳米柿球尺寸大小决定其光学性质的不同。
(3)采用简单无机盐助合成的水热体系,通过稀土硝酸化合物和氟化钠反应制备了不同化学组成和形貌的稀土氟化物纳米材料,如Na(Y1.5Na0.5)F6纳米梭、α-NaYF4纳米球、YF3八面体等。对反应条件(反应温度、反应时间、盐的浓度和其他轻稀土氟化物等)的研究表明:盐不仅能控制反应速度,还有控制产物物相的作用;盐选择性控制晶体不同晶面的生长,从而达到控制产物形貌的作用。此外研究还表明稀土离子半径对产物的形成和形貌也有重要的影响。
(4)用两个反应体系合成出具有不同形貌的CeO2,并分别讨论不同反应体系对产物的影响。一、采用简单甲苯溶剂热方法,用无机盐作反应前驱物,十六胺作表面活性剂,合成出单分散的CeO2立方体,并研究了不同粒径CeO2的电学和光催化性质。通过对反应条件(水量、脂肪胺与铈源的摩尔比、以及脂肪胺的链长)研究,结果表明晶体固有的生长特性和表面活性剂对晶面的选择性吸附是形成CeO2立方体的关键因素。二、采用自模板牺牲法,通过简单有机络合剂水热反应合成出CeCO3OH菱角组装体,我们认为:CeCO3OH菱角组装体是由晶体各向异性和络合剂对晶面选择性吸附决定的,而外部生长条件(反应时间、络合剂/Ce3+的摩尔比、温度等)也影响产物的形貌。高温氧化分解成(自模板牺牲法)CeO2菱角组装体。
Due to their novel optical, electronic and magnetic properties, nano/micro- materials of lanthanide compounds have great potential applications in many fields, such as photoluminescence, optical fibers, humidity sensors, catalysts, magnetic materials and antibacterial materials. Stimulated by both the promising application and the interesting properties, much attention has been devoted to the controlled synthesis of lanthanide nanomaterials with different morphologies and the investigation of their size/shape-dependent properties. On the other hand, the abundant resource of rare earth in our country enables us to extend the applications of lanthanide nanomaterials in the above mentioned fields. In this work, a series of nano/micro-materials of lanthanide with uniform size and morphology have been successfully synthesized via a solution route. The main contents of this thesis are summarized as following:
(1) LnPO4·nH2O (Ln = La-Gd) (n = 0～1) and Ln(OH)3 (Ln = La-Gd) one-dimensional nanomaterials are fabricated without using any surfactant or template at room temperature. The formation of one-dimensional nanomaterials can be attributed to the anisotropic growth of light lanthanide phosphate and light lanthanide hydroxide. The aspect ratios of one-dimensional nanomaterials can be effectively controlled by adjusting the reaction time and pH value of the reaction system. Under the similar reaction conditions, the monoclinic YPO4·2H2O and Eu3+-doped LaPO4 nanowires are also obtained. The optical properties of the doped nanomaterials prepared at different reaction time and Eu(OH)3 are related to the morphology and the crystalline degree. The light lanthanide not only have similar chemical property and shape but also demonstrate own unique character.
(2) Monodisperse YVO4 (DyVO4, ErVO4) architectures with persimmon-like, cube-like and nanoparticle shape have been synthesized via a complexing agent-assisted solution route. The shape and size of these as-prepared architectures can be tuned effectively by controlling the reaction conditions, such as reaction time, the molar ratio of complexing agent/Y3+, the structure of the complexing agent and rare earth precurors. As a typical morphology, the growth process of monodisperse nanopersimmons has been examined. The interaction between rare earth ion and the complexing agent is crucial for the morphology of the as-synthesized lanthanide orthovanadate. The optical properties of YVO4 nanopersimmons are relevant to their size and shape.
(3) The different kinds of yttrium fluoride have been prepared via a simple hydrothermal method in the presence of sodium nitrate. The morphology and chemical composition of the as-obtained product can be controlled by varying factors, such as the concentration of the starting salt in solution, the temperature and reaction time and rare earth precursors. The product composition variation from Na(Y1.5Na0.5)F6 andα-NaYF4 to YF3, and corresponding morphological transformation from spherical aggregation to octahedron have been observed under the different reaction conditions. Further studies reveal that the morphology and composition of the as-synthesized lanthanide fluoride are also determined by the ionic radius of rare earth. It is reasonable to believe that sodium nitrate plays double roles in the reaction. One is to serve as chelating ligand to kinetically control the reaction rate, and the other is to act as surfactant to affect the facet growth and the shape of the product.
(4) Different ceria morphologies have been obtained with two reaction system. First,cubic-like CeO2 nanocrystals have been synthesized through a facile solvothermal process in toluene using hexadecylamine as capping agent and CeCl3·7H2O as precursor. The water content, the concentration of ligand and the structure of the aliphatic amine are critical to the formation of the monodisperse nanocub. The growth of ceria nanocubes is strongly dependent on the intrinsic crystal structure and the kinetic factors employed during the synthetic course. The electrochemical properties of the obtained samples reveal its potential application as anode material in lithium-ion batteries. The photocatalytic properties of the obtained samples present the size/shape-dependent properties. Second, Monodisperse CeCO3OH architectures with water caltrop-like shape have been synthesized by a complexing agent-assisted solution route. The anisotropic growth of light CeCO3OH and a complexing agent have great influence on the formation of architectures. The shape and size of CeCO3OH architectures can be controlled effectively by adjusting the reaction conditions, such as reaction time, the molar ratio of complexing agent/Ce3+ and reaction temperature. Ceria (CeO2) architectures with caltrop-like shape have been obtained by a thermal decomposition oxidation process at high temperature using as-synthesized CeCO3OH.
(1)在无表面活性剂或模板剂的条件下,室温水相反应体系成功地合成出系列轻稀土磷酸盐LnPO4·nH2O(Ln=La-Gd)(n=0～1)和氢氧化物Ln(OH)3(Ln=La-Gd)一维纳米材料。一维纳米材料的形成主要是由六方晶相结构的轻稀土磷酸盐和氢氧化物的各向异性所决定的,它的长径比还与反应体系的pH值和反应时间有关。并研究不同长度Eu3+:LaPO4纳米线和Eu(OH)3纳米棒的室温光学性质,我们发现纳米线的发光强度与结晶度和形貌有关。研究表明:轻稀土化合物具有类似的化学性质和形貌,但也有展示独特的个性(如在同样的实验条件,我们合成出重稀土单斜相YPO4·2H2O纳米线的合成)。
(2)以有机络合剂辅助合成的水热体系,通过简单的稀土硝酸化合物与原钒酸钠反应合成出多种多级组装结构的重稀土钒酸盐化合物(YVO4、DyVO4、ErVO4)纳米材料,如纳米柿球、纳米立方体组装结构和纳米粒子等,并对纳米柿球的组装结构形成机理进行了较为系统的研究。研究表明:反应时间、稀土离子与络合剂摩尔比、络合剂的种类以及稀土离子的半径对重稀土钒酸盐的组装结构均具有重要的影响;纳米柿球尺寸大小决定其光学性质的不同。
(3)采用简单无机盐助合成的水热体系,通过稀土硝酸化合物和氟化钠反应制备了不同化学组成和形貌的稀土氟化物纳米材料,如Na(Y1.5Na0.5)F6纳米梭、α-NaYF4纳米球、YF3八面体等。对反应条件(反应温度、反应时间、盐的浓度和其他轻稀土氟化物等)的研究表明:盐不仅能控制反应速度,还有控制产物物相的作用;盐选择性控制晶体不同晶面的生长,从而达到控制产物形貌的作用。此外研究还表明稀土离子半径对产物的形成和形貌也有重要的影响。
(4)用两个反应体系合成出具有不同形貌的CeO2,并分别讨论不同反应体系对产物的影响。一、采用简单甲苯溶剂热方法,用无机盐作反应前驱物,十六胺作表面活性剂,合成出单分散的CeO2立方体,并研究了不同粒径CeO2的电学和光催化性质。通过对反应条件(水量、脂肪胺与铈源的摩尔比、以及脂肪胺的链长)研究,结果表明晶体固有的生长特性和表面活性剂对晶面的选择性吸附是形成CeO2立方体的关键因素。二、采用自模板牺牲法,通过简单有机络合剂水热反应合成出CeCO3OH菱角组装体,我们认为:CeCO3OH菱角组装体是由晶体各向异性和络合剂对晶面选择性吸附决定的,而外部生长条件(反应时间、络合剂/Ce3+的摩尔比、温度等)也影响产物的形貌。高温氧化分解成(自模板牺牲法)CeO2菱角组装体。
Due to their novel optical, electronic and magnetic properties, nano/micro- materials of lanthanide compounds have great potential applications in many fields, such as photoluminescence, optical fibers, humidity sensors, catalysts, magnetic materials and antibacterial materials. Stimulated by both the promising application and the interesting properties, much attention has been devoted to the controlled synthesis of lanthanide nanomaterials with different morphologies and the investigation of their size/shape-dependent properties. On the other hand, the abundant resource of rare earth in our country enables us to extend the applications of lanthanide nanomaterials in the above mentioned fields. In this work, a series of nano/micro-materials of lanthanide with uniform size and morphology have been successfully synthesized via a solution route. The main contents of this thesis are summarized as following:
(1) LnPO4·nH2O (Ln = La-Gd) (n = 0～1) and Ln(OH)3 (Ln = La-Gd) one-dimensional nanomaterials are fabricated without using any surfactant or template at room temperature. The formation of one-dimensional nanomaterials can be attributed to the anisotropic growth of light lanthanide phosphate and light lanthanide hydroxide. The aspect ratios of one-dimensional nanomaterials can be effectively controlled by adjusting the reaction time and pH value of the reaction system. Under the similar reaction conditions, the monoclinic YPO4·2H2O and Eu3+-doped LaPO4 nanowires are also obtained. The optical properties of the doped nanomaterials prepared at different reaction time and Eu(OH)3 are related to the morphology and the crystalline degree. The light lanthanide not only have similar chemical property and shape but also demonstrate own unique character.
(2) Monodisperse YVO4 (DyVO4, ErVO4) architectures with persimmon-like, cube-like and nanoparticle shape have been synthesized via a complexing agent-assisted solution route. The shape and size of these as-prepared architectures can be tuned effectively by controlling the reaction conditions, such as reaction time, the molar ratio of complexing agent/Y3+, the structure of the complexing agent and rare earth precurors. As a typical morphology, the growth process of monodisperse nanopersimmons has been examined. The interaction between rare earth ion and the complexing agent is crucial for the morphology of the as-synthesized lanthanide orthovanadate. The optical properties of YVO4 nanopersimmons are relevant to their size and shape.
(3) The different kinds of yttrium fluoride have been prepared via a simple hydrothermal method in the presence of sodium nitrate. The morphology and chemical composition of the as-obtained product can be controlled by varying factors, such as the concentration of the starting salt in solution, the temperature and reaction time and rare earth precursors. The product composition variation from Na(Y1.5Na0.5)F6 andα-NaYF4 to YF3, and corresponding morphological transformation from spherical aggregation to octahedron have been observed under the different reaction conditions. Further studies reveal that the morphology and composition of the as-synthesized lanthanide fluoride are also determined by the ionic radius of rare earth. It is reasonable to believe that sodium nitrate plays double roles in the reaction. One is to serve as chelating ligand to kinetically control the reaction rate, and the other is to act as surfactant to affect the facet growth and the shape of the product.
(4) Different ceria morphologies have been obtained with two reaction system. First,cubic-like CeO2 nanocrystals have been synthesized through a facile solvothermal process in toluene using hexadecylamine as capping agent and CeCl3·7H2O as precursor. The water content, the concentration of ligand and the structure of the aliphatic amine are critical to the formation of the monodisperse nanocub. The growth of ceria nanocubes is strongly dependent on the intrinsic crystal structure and the kinetic factors employed during the synthetic course. The electrochemical properties of the obtained samples reveal its potential application as anode material in lithium-ion batteries. The photocatalytic properties of the obtained samples present the size/shape-dependent properties. Second, Monodisperse CeCO3OH architectures with water caltrop-like shape have been synthesized by a complexing agent-assisted solution route. The anisotropic growth of light CeCO3OH and a complexing agent have great influence on the formation of architectures. The shape and size of CeCO3OH architectures can be controlled effectively by adjusting the reaction conditions, such as reaction time, the molar ratio of complexing agent/Ce3+ and reaction temperature. Ceria (CeO2) architectures with caltrop-like shape have been obtained by a thermal decomposition oxidation process at high temperature using as-synthesized CeCO3OH.
引文
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