配合物为前驱体的多孔稀土氧化物制备与表征
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摘要
稀土氧化物材料,如二氧化铈、氧化镧、氧化钇等,因其在光学、催化、热学等方面的优异性能受到人们的广泛关注。近年来不同形貌和纳米结构的稀土氧化物材料被合成并见诸报道,例如稀土氧化物胶体微球、薄膜、纳米颗粒、纳米管、纳米棒或者三维大孔材料等。考虑到稀土氧化物材料的优异性能,合成具有新形貌和纳米结构的稀土氧化物材料,发展简便并适用广泛的制备方法具有重要的理论和实际意义。
本文主要研究以水热方法合成一系列不同形貌的稀土配位聚合物材料,并以此为前驱体,通过焙烧合成相应的稀土氧化物纳米结构材料。本文使用X-射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、核磁共振(NMR)、红外光谱(IR)、氮气吸附和元素分析(EA)等表征手段对所得材料进行了详细表征。同时仔细研究了各种前驱体的生成机理和形貌控制条件,并应用这一方法合成了一系列掺杂型稀土固溶体氧化物材料。本文的主要内容有以下三部分：
1)稀土-天冬酰胺配位聚合物大孔、微球及空心球材料及其相应稀土氧化物材料的合成。
通过天冬酰胺与稀土离子在水热条件下反应,以自下而上(bottom-up)的无模板方式合成了一系列稀土配位聚合物材料,包括：具有取向大孔或多级结构大孔的块体材料,分散性良好的实心微球或者空心微球材料,其中大孔和空心球配位聚合物材料系首次报道。通过对跟踪实验的详细表征,证实了这些配位聚合物材料的生成过程均遵循Ostwald熟化规律,配位聚合物材料中有机配体所占的比例决定了材料的形貌和生成过程。而且通过这一方法,还可以获得稀土-稀土以及过渡金属-稀土掺杂型的配位聚合物大孔及微球材料。
以所制备的配位聚合物材料为前驱体,通过在空气中焙烧热解,可以进一步获得相应的稀土氧化物材料,包括：具有多级孔结构的稀土氧化物材料,由纳米颗粒聚集而成的壳核型或实心微球材料,具有纳米孔壁的空壳球材料以及多种掺杂型稀土氧化物固溶体材料。紫外-可见漫反射谱和荧光谱测试用来表征了部分氧化物材料的光学性能。
这一无模板和自下而上的组装方法体现了金属—配体相互作用与组装的高度可调性,并为合成其它成分和形貌可调的金属氧化物提供了新的有效途径。
2)草酸根阴离子与氨基酸竞争作用调控下制备稀土基前驱体材料及其相应的稀土氧化物材料。
通过稀土阳离子、草酸根阴离子、谷氨酰胺或者天冬酰胺在水热条件下的反应合成了稀土基前驱体化合物,包括纤维束或三维大孔材料。将这些前驱体化合物在空气中焙烧即获得了相应的稀土氧化物材料,这些氧化物材料很好的保持了其前驱体的微观形貌,而且焙烧后生成的氧化物颗粒堆积构筑形成了多孔结构。
尽管天冬酰胺和谷氨酰胺的结构比较相近,在水热条件下,它们与稀土阳离子的络合相互作用能力却表现出了很大的差异,这一点可由ESI-MS(电喷雾质谱)的检测在分子水平上获得了证实。对于谷氨酰胺而言,它与稀土阳离子的络合作用弱于稀土阳离子和草酸根阴离子的静电相互作用力。因此,当反应体系中使用谷氨酰胺做为添加剂时,所得的前驱体材料为结晶的草酸盐纳米纤维束。然而,对于天冬酰胺,它与稀土阳离子的络合作用强于静电作用力,因此在它的反应体系中,所获得的前驱体材料是具有三维大孔结构的无定形配合物。
基于天冬酰胺和草酸根离子对于稀土阳离子的竞争性相互作用,通过改变草酸根浓度和反应溶液pH值的方式,可以方便地调节所得前驱体材料的形貌,例如：获得了具有不同孔隙率的大孔材料,具有两种孔径分布的大孔材料和由菱形纳米片组成的面包状颗粒等。
将这些前驱体材料在空气中焙烧后,获得了保持其前驱体形貌的多孔稀土氧化物材料。这一部分内容表明有机分子与金属阳离子络合能力的强弱可能是它们实现对于金属盐前驱体形貌控制的关键因素。
3)以EDTA为配体合成了一系列结晶稀土配位聚合物材料及其相应的稀土氧化物材料。
在水热条件下,EDTA可以与多种稀土阳离子形成结晶稀土配体聚合物材料,这些稀土配位聚合物材料具有纳米纤维和微片两类形貌。与前述各种无定形配位聚合物不同的是,结晶配位聚合物可以通过EA,XPS,TGA等测试手段的综合应用,明确得出表示其成分的化学式。跟踪实验证实了EDTA配位聚合物材料的形成过程遵循Ostwald熟化规律。
以EDTA为配体还可以合成稀土—稀土,稀土—过渡金属配位聚合物材料,值得注意的是这些掺杂型配位聚合物材料的形貌与结构和掺杂金属的种类,浓度具有明显的相关性。例如：锰-镧配位聚合物微片,随着锰所占比例(摩尔量)的增加,所得微片材料的尺寸明显减小。
将这些结晶配位聚合物材料在空气中焙烧,即可进一步获得相应的多孔稀土氧化物纤维、微片材料。在焙烧所得的样品中,大部分较好的保持了前驱体的形貌。
Lanthanide oxides and mixed oxides such as:ceria, lanthanum oxide, yttria etc., have wide applications due to their luminescent, catalytic and thermal properties. As a result, different morphologies of colloid spheres, thin films, nanoparticles, nanotubes, nanorods or microrods, and 3D-macroporous materials have been reported in recent years. Considering excellent properties of lanthanide oxides, It is very important to fabricate lanthanide oxides with novel morphology and structure using simple and universal synthetic method.
In this dissertation, we focus on a bottom-up, template-free fabrication of a series lanthanide based precursors and their corresponding lanthanide oxides. By a facile hydrothermal reaction with lanthanide ions and organic ligands e.g.:amino acids, lathandie based metal-organic compounds could be prepared, and with these compounds as precursors, lanthanide oxides were obtained by calcination. The products were carefully characterized by various methods, including Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared spectroscopy (FT-IR)^ X-Ray Powder Diffraction (XRD), N2 adsorption-desorption, UV-Vis diffuse reflection spectroscopy, Thermo Gravimetric-Differential Thermal Analysis (TG-DTA) and X-ray Photoelectron Spectroscopy (XPS), Elemental analysis(EA) etc., and the formation mechanisms and morphology control factors were studied in detail meanwhile. Moreover, series of doped lanthanide oxide solid solution were also prepared using this method. The main content of the thesis is composed of the following three parts:
1) A series of unique lanthanide-organic coordination polymer products were fabricated by a bottom-up and template-free method of hydrothermal reaction with lanthanide ions and asparagine. The as-prepared products included macroporous foam with aligned or hierarchical macropores, dispersed microspheres and hollow spheres, among them, the macroporous foam and hollow spheres coordination polymers were first reported.
From the time-dependent experiments of all the as-synthesized coordination polymers, it is proved that the formation mechanisms of these products were Ostwald ripening process, and organic content of coordination polymers was found as the key point for the morphology and the formation process of the products. Moreover, using this template free method, lanthanide mixed coordination polymers and transition metal doped lanthanide coordination polymers could also be prepared.
Furthermore, with these coordination polymer products as precursors, corresponding lanthanide oxides were obtained after calcination, such as hierarchical meso-macroporous lanthanide oxides foams, core-shell microspheres assembled by nanoparticles, hollow spheres with porous walls and many kinds of doped lanthanide oxides materials. Among them, some products with luminescent properties were test using UV-Vis and Fluorescence instruments.
Our work displays the extensive tailorability of metal-ligand interaction, and may open up new possibilities for the fabrication of metal oxides with well-defined morphologies and diverse compositions.
2) Lanthanide based precursors (including nanofibers and 3D-macroporous foam) were synthesized by a hydrothermal reaction with lanthanide salts, sodium oxalate and asparagine (or glutamine). With these compounds as precursors, lanthanide oxides were obtained after calcination which remained the morphology of their precursors. Moreover, assembled nanoparticles gave rise to a porous structure for these lanthanide oxides materials.
Although asparagine and glutamine have similar structure, they exhibited greatly different complexation abilities with lanthanide cations, and this point was further confirmed by ESI-MS detection at the molecular level。For glutamine, its complex ability with lanthanide cations was weaker than the electrostatic interactions between oxalate anions and lanthanide cations. So when using glutamine, the as-prepared product was crystalline oxalate nanofibers. While for asparagine, its complex ability with lanthanide cations was stronger than the electrostatic interaction. So when using asparagine, the product was amorphous lanthanide organic precursors with 3D macroporous structures.
Variation of oxalate anion concentration or the pH value of the reaction solution could tune the morphology of the products, e.g.:macroporous foams with tunable porosity, macroprous foam with bimodal macropores and microparticles assembled by rhombic nanoplates were prepared.
With these compounds as precursors, porous lanthanide oxides were obtained which remained the morphology of their precursors. Our work suggests that the complexation ability of organic molecules with metal cations could be a crucial factor for morphological control of the precursors.
3) Crystalline lanthanide coordination polymers including nanofibers and microflakes were fabricated under hydrothermal conditions with EDTA and lanthanide cations. Time dependent experiments were performed and it is proved that the formation mechanism of these crystalline coordination polymers was Ostwald ripening. Here the chemical compositions of coordination polymers could be calculated assisted by EA, XPS and TGA test.
Moreover, this method was expanded to prepare lanthanide-lanthanide and lanthanide-transition metal coordination polymers. It is interesting to note that different doped metal cations and their quantity could influence the morphology of as-prepared products. For example, the size of Mn-La microflakes was decreased when the doped Mn cations increased.
Furthermore, porous lanthanide oxides nanofibers and microflakes could be obtained by thermolysis of their corresponding precursors. However, minor lanthanide oxides could not remain the morphology of their precursors after calcination, and this problem should be solved in future in our lab.
本文主要研究以水热方法合成一系列不同形貌的稀土配位聚合物材料,并以此为前驱体,通过焙烧合成相应的稀土氧化物纳米结构材料。本文使用X-射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、核磁共振(NMR)、红外光谱(IR)、氮气吸附和元素分析(EA)等表征手段对所得材料进行了详细表征。同时仔细研究了各种前驱体的生成机理和形貌控制条件,并应用这一方法合成了一系列掺杂型稀土固溶体氧化物材料。本文的主要内容有以下三部分：
1)稀土-天冬酰胺配位聚合物大孔、微球及空心球材料及其相应稀土氧化物材料的合成。
通过天冬酰胺与稀土离子在水热条件下反应,以自下而上(bottom-up)的无模板方式合成了一系列稀土配位聚合物材料,包括：具有取向大孔或多级结构大孔的块体材料,分散性良好的实心微球或者空心微球材料,其中大孔和空心球配位聚合物材料系首次报道。通过对跟踪实验的详细表征,证实了这些配位聚合物材料的生成过程均遵循Ostwald熟化规律,配位聚合物材料中有机配体所占的比例决定了材料的形貌和生成过程。而且通过这一方法,还可以获得稀土-稀土以及过渡金属-稀土掺杂型的配位聚合物大孔及微球材料。
以所制备的配位聚合物材料为前驱体,通过在空气中焙烧热解,可以进一步获得相应的稀土氧化物材料,包括：具有多级孔结构的稀土氧化物材料,由纳米颗粒聚集而成的壳核型或实心微球材料,具有纳米孔壁的空壳球材料以及多种掺杂型稀土氧化物固溶体材料。紫外-可见漫反射谱和荧光谱测试用来表征了部分氧化物材料的光学性能。
这一无模板和自下而上的组装方法体现了金属—配体相互作用与组装的高度可调性,并为合成其它成分和形貌可调的金属氧化物提供了新的有效途径。
2)草酸根阴离子与氨基酸竞争作用调控下制备稀土基前驱体材料及其相应的稀土氧化物材料。
通过稀土阳离子、草酸根阴离子、谷氨酰胺或者天冬酰胺在水热条件下的反应合成了稀土基前驱体化合物,包括纤维束或三维大孔材料。将这些前驱体化合物在空气中焙烧即获得了相应的稀土氧化物材料,这些氧化物材料很好的保持了其前驱体的微观形貌,而且焙烧后生成的氧化物颗粒堆积构筑形成了多孔结构。
尽管天冬酰胺和谷氨酰胺的结构比较相近,在水热条件下,它们与稀土阳离子的络合相互作用能力却表现出了很大的差异,这一点可由ESI-MS(电喷雾质谱)的检测在分子水平上获得了证实。对于谷氨酰胺而言,它与稀土阳离子的络合作用弱于稀土阳离子和草酸根阴离子的静电相互作用力。因此,当反应体系中使用谷氨酰胺做为添加剂时,所得的前驱体材料为结晶的草酸盐纳米纤维束。然而,对于天冬酰胺,它与稀土阳离子的络合作用强于静电作用力,因此在它的反应体系中,所获得的前驱体材料是具有三维大孔结构的无定形配合物。
基于天冬酰胺和草酸根离子对于稀土阳离子的竞争性相互作用,通过改变草酸根浓度和反应溶液pH值的方式,可以方便地调节所得前驱体材料的形貌,例如：获得了具有不同孔隙率的大孔材料,具有两种孔径分布的大孔材料和由菱形纳米片组成的面包状颗粒等。
将这些前驱体材料在空气中焙烧后,获得了保持其前驱体形貌的多孔稀土氧化物材料。这一部分内容表明有机分子与金属阳离子络合能力的强弱可能是它们实现对于金属盐前驱体形貌控制的关键因素。
3)以EDTA为配体合成了一系列结晶稀土配位聚合物材料及其相应的稀土氧化物材料。
在水热条件下,EDTA可以与多种稀土阳离子形成结晶稀土配体聚合物材料,这些稀土配位聚合物材料具有纳米纤维和微片两类形貌。与前述各种无定形配位聚合物不同的是,结晶配位聚合物可以通过EA,XPS,TGA等测试手段的综合应用,明确得出表示其成分的化学式。跟踪实验证实了EDTA配位聚合物材料的形成过程遵循Ostwald熟化规律。
以EDTA为配体还可以合成稀土—稀土,稀土—过渡金属配位聚合物材料,值得注意的是这些掺杂型配位聚合物材料的形貌与结构和掺杂金属的种类,浓度具有明显的相关性。例如：锰-镧配位聚合物微片,随着锰所占比例(摩尔量)的增加,所得微片材料的尺寸明显减小。
将这些结晶配位聚合物材料在空气中焙烧,即可进一步获得相应的多孔稀土氧化物纤维、微片材料。在焙烧所得的样品中,大部分较好的保持了前驱体的形貌。
Lanthanide oxides and mixed oxides such as:ceria, lanthanum oxide, yttria etc., have wide applications due to their luminescent, catalytic and thermal properties. As a result, different morphologies of colloid spheres, thin films, nanoparticles, nanotubes, nanorods or microrods, and 3D-macroporous materials have been reported in recent years. Considering excellent properties of lanthanide oxides, It is very important to fabricate lanthanide oxides with novel morphology and structure using simple and universal synthetic method.
In this dissertation, we focus on a bottom-up, template-free fabrication of a series lanthanide based precursors and their corresponding lanthanide oxides. By a facile hydrothermal reaction with lanthanide ions and organic ligands e.g.:amino acids, lathandie based metal-organic compounds could be prepared, and with these compounds as precursors, lanthanide oxides were obtained by calcination. The products were carefully characterized by various methods, including Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared spectroscopy (FT-IR)^ X-Ray Powder Diffraction (XRD), N2 adsorption-desorption, UV-Vis diffuse reflection spectroscopy, Thermo Gravimetric-Differential Thermal Analysis (TG-DTA) and X-ray Photoelectron Spectroscopy (XPS), Elemental analysis(EA) etc., and the formation mechanisms and morphology control factors were studied in detail meanwhile. Moreover, series of doped lanthanide oxide solid solution were also prepared using this method. The main content of the thesis is composed of the following three parts:
1) A series of unique lanthanide-organic coordination polymer products were fabricated by a bottom-up and template-free method of hydrothermal reaction with lanthanide ions and asparagine. The as-prepared products included macroporous foam with aligned or hierarchical macropores, dispersed microspheres and hollow spheres, among them, the macroporous foam and hollow spheres coordination polymers were first reported.
From the time-dependent experiments of all the as-synthesized coordination polymers, it is proved that the formation mechanisms of these products were Ostwald ripening process, and organic content of coordination polymers was found as the key point for the morphology and the formation process of the products. Moreover, using this template free method, lanthanide mixed coordination polymers and transition metal doped lanthanide coordination polymers could also be prepared.
Furthermore, with these coordination polymer products as precursors, corresponding lanthanide oxides were obtained after calcination, such as hierarchical meso-macroporous lanthanide oxides foams, core-shell microspheres assembled by nanoparticles, hollow spheres with porous walls and many kinds of doped lanthanide oxides materials. Among them, some products with luminescent properties were test using UV-Vis and Fluorescence instruments.
Our work displays the extensive tailorability of metal-ligand interaction, and may open up new possibilities for the fabrication of metal oxides with well-defined morphologies and diverse compositions.
2) Lanthanide based precursors (including nanofibers and 3D-macroporous foam) were synthesized by a hydrothermal reaction with lanthanide salts, sodium oxalate and asparagine (or glutamine). With these compounds as precursors, lanthanide oxides were obtained after calcination which remained the morphology of their precursors. Moreover, assembled nanoparticles gave rise to a porous structure for these lanthanide oxides materials.
Although asparagine and glutamine have similar structure, they exhibited greatly different complexation abilities with lanthanide cations, and this point was further confirmed by ESI-MS detection at the molecular level。For glutamine, its complex ability with lanthanide cations was weaker than the electrostatic interactions between oxalate anions and lanthanide cations. So when using glutamine, the as-prepared product was crystalline oxalate nanofibers. While for asparagine, its complex ability with lanthanide cations was stronger than the electrostatic interaction. So when using asparagine, the product was amorphous lanthanide organic precursors with 3D macroporous structures.
Variation of oxalate anion concentration or the pH value of the reaction solution could tune the morphology of the products, e.g.:macroporous foams with tunable porosity, macroprous foam with bimodal macropores and microparticles assembled by rhombic nanoplates were prepared.
With these compounds as precursors, porous lanthanide oxides were obtained which remained the morphology of their precursors. Our work suggests that the complexation ability of organic molecules with metal cations could be a crucial factor for morphological control of the precursors.
3) Crystalline lanthanide coordination polymers including nanofibers and microflakes were fabricated under hydrothermal conditions with EDTA and lanthanide cations. Time dependent experiments were performed and it is proved that the formation mechanism of these crystalline coordination polymers was Ostwald ripening. Here the chemical compositions of coordination polymers could be calculated assisted by EA, XPS and TGA test.
Moreover, this method was expanded to prepare lanthanide-lanthanide and lanthanide-transition metal coordination polymers. It is interesting to note that different doped metal cations and their quantity could influence the morphology of as-prepared products. For example, the size of Mn-La microflakes was decreased when the doped Mn cations increased.
Furthermore, porous lanthanide oxides nanofibers and microflakes could be obtained by thermolysis of their corresponding precursors. However, minor lanthanide oxides could not remain the morphology of their precursors after calcination, and this problem should be solved in future in our lab.
引文
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