稀土含氮配位聚合物微纳米结构的合成、表征及性能研究

发布时间：2018-03-19 14:44

本文选题：配位聚合物　切入点：微纳米材料　出处：《江西师范大学》2016年硕士论文　论文类型：学位论文

【摘要】：配位聚合物微/纳米材料是一种新型的材料,在光学、磁性、催化、生物分析等许多领域有广泛的应用前景。研究稀土配位聚合微/纳米材料的合成方法,探讨其结构和形貌控制机理,挖掘其潜在的应用等具有重要的意义。为此,本论文以含氮配体的配合物为研究对象,采用溶剂热和微波-水热的合成方法,制备出了以钆基配位聚合物为核,铕基配位聚合物为壳的核壳结构纳米球;钆基配位聚合物空心纳米球;钇基配位聚合物微米球。考察了不同反应条件对产物的影响,综合运用了多种测试手段对产物进行表征。在其应用的研究方面,主要研究了产物的发光性能,磁性和造影剂方面。本研究工作为其它配位聚合物的研究提供了理论依据和方法路线。本论文的主要研究内容有:(1)配位聚合物核壳结构的合成、表征及上、下转换发光采用简单、方便的水热和溶剂热合成方法,以尿囊素为配体,在没有其他模板剂的条件下,合成了以钆基配位聚合物为核,铕基配位聚合物为壳的核壳结构。同时,对核壳结构进行了上下转换发光的测试,研究表明壳的引入能增强上转换发光强度,并且具备下转换发光性能。T1加权成像测试结果表明,配位聚合物核壳结构有明显的T1成像规律。(2)钆基配位聚合物空心结构的合成与表征及性能研究以双甘氨肽为配体,Gd~(3+)为中心离子,掺杂Yb~(3+)和Er~(3+),通过控制反应的溶剂、温度和时间,采用溶剂热的方法合成了大小均一空心结构的配位聚合物纳米球。通过高温煅烧后,形成的钆基配位聚合物空心球转会换成了Gd_2O_3。采用一系列的表征手段对产品进行表征。同时,对配位聚合物空心纳米球进行了磁性测试和上转换测试,研究表明样品具备上转换发光性能。使用核磁共振分析软件测出弛豫信息,对产品进行T1加权成像,讨论了配位聚合物空心纳米球作为造影剂的性能。(3)钇基配位聚合物微米球的合成与表征及发光性能研究采用的是微波-水热的方法,以天门冬酰胺为配体,通过控制温度和不同Eu~(3+)的浓度,合成了具有荧光性能的配位聚合物。研究了产物不同温度的荧光寿命,不同掺杂比例的荧光强度,不同温度的荧光强度。实验结果表明,当掺杂Eu~(3+)的量是5%时,荧光强度最强,随着浓度增加,荧光淬灭,低温条件下配位聚合物微米球的有更长的荧光寿命和更强的荧光强度,并且温度越低,荧光强度越强,具有荧光温敏的特性。
[Abstract]:Coordination polymer micro/ nanomaterials are a new type of materials, which have been widely used in many fields, such as optics, magnetism, catalysis, biological analysis, etc. The synthesis methods of rare earth coordination polymerized micro / nano materials have been studied. It is of great significance to study the structure and morphology control mechanism and explore its potential applications. In this paper, the complexes of nitrogen-containing ligands were studied, and the synthesis methods of solvothermal and microwave-hydrothermal methods were adopted. Core-shell structure nanospheres with gadolinium based coordination polymer as core, europium based coordination polymer as shell, gadolinium based coordination polymer hollow nanospheres, yttrium based coordination polymer microspheres were prepared. The effects of different reaction conditions on the products were investigated. In the aspect of its application, the luminescence property of the product was studied. Magnetic and contrast agents. This work provides a theoretical basis and method for the study of other coordination polymers. The main content of this thesis is the synthesis, characterization and characterization of the core-shell structure of coordination polymers. In this paper, a simple and convenient hydrothermal and solvothermal synthesis method for downconversion luminescence was used to synthesize the core-shell structure with gadolinium based coordination polymer as core and europium based coordination polymer as shell, using allantoin as ligand and without other templates. The upper and lower conversion luminescence of core-shell structure is tested. The results show that the introduction of shell can enhance the intensity of up-conversion luminescence, and has downconversion luminescence property. T1 weighted imaging results show that, Synthesis, characterization and Properties of Gadolinium based Coordination Polymer Hollow structure with clear T1 Imaging characteristics of Coordination Polymer Core-shell structure; using diglycine peptide as the ligand Gdfen 3) as the central ion, doped with Yb~(3) and Er~(3, the solvent of the reaction was controlled. Coordination polymer nanospheres with homogeneous hollow structure were synthesized by solvothermal method at temperature and time. The gadolinium coordination polymer hollow spheres were transferred to Gd _ 2O _ 3. The products were characterized by a series of characterization methods. At the same time, magnetic and up-conversion tests were performed on the coordination polymer hollow spheres. The results show that the samples have upconversion luminescence properties. The relaxation information is measured by nuclear magnetic resonance analysis software, and the products are used for T1 weighted imaging. The synthesis and characterization of yttrium based coordination polymer microspheres and their luminescent properties were discussed. The microwave-hydrothermal method with asparagine as ligand was used to study the photoluminescence properties of yttrium coordination polymer microspheres. The coordination polymers with fluorescence properties were synthesized by controlling the temperature and the concentration of Eu~(3). The fluorescence lifetime of the product at different temperature, the fluorescence intensity of different doping ratio and the fluorescence intensity at different temperature were studied. When the amount of doped Eu~(3) is 5, the fluorescence intensity is the strongest. With the increase of concentration, fluorescence quenching, the coordination polymer microspheres have longer fluorescence lifetime and stronger fluorescence intensity at low temperature, and the lower the temperature, the stronger the fluorescence intensity. It has the characteristic of fluorescence temperature sensitivity.
【学位授予单位】：江西师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O641.4

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