论文总字数：17769字

摘 要

随着近年来各领域科学技术的的不断革新，上转换纳米凭借其自身的优越性，得到了广泛应用。随着人们对上转换材料的一步步深入研究，其发展跟应用以及性能的修饰成为了各研究者关注的焦点。我们能在很多的领域找到上转换材料的踪迹，比如医学、生物学、分析化学等等。我们熟悉的有机染料、量子点以及荧光素、荧光蛋白的都是比较久远的荧光探针，它们的发射光位于紫外区或者是可见光的区域，会产生很强的背景干扰，且对于所研究的样本有很强破坏性，不适应医学或是生物学的研究。而上转换的纳米材料可以解决传统发光材料的弊端，使其在更广的范围中得以应用。还有，上转换纳米材料的毒副作用很小，对于生物体示踪研究有很大帮助，解决了传统材料存在的安全隐患问题。综上所述，对于上转换材料的研究需要更进一步，是的合成方法以及合成的条件更加完善，可以实现大规模的复制上产，从而使其运用范围拓宽。

本论文是利用溶剂法制备掺杂稀土离子的上转换发光材料，并将其外部的油溶性物质改变，从而增加水溶性,利用的方法是环糊精包覆方法和介孔SiO₂包覆。用荧光分析法来分析所合成的纳米粒子，得到相关可利用的信息，为进一步的研究做准备。

关键词：稀土离子 上转换 溶剂法 表面修饰

Preparation of Near Infrared Excited Upconversion Nanoparticles by Water - soluble Modified Rare Earth Nanocrystals

Abstract

With the continuous innovation of science and technology in various fields in recent years, the conversion of nano by virtue of its own superiority, has been widely used. With the people on the conversion of materials step by step in-depth study, its development and application and performance modification has become the focus of attention of the researchers. We can find traces of upconversion materials in many areas, such as medicine, biology, analytical chemistry, and so on. We are familiar with organic dyes, quantum dots and fluorescein, fluorescent protein are relatively long fluorescent probe, their emission light is located in the ultraviolet region or visible light area, will have a strong background interference, and for the study The samples are highly destructive and do not fit in medical or biology research. The upconversion of nano-materials can solve the drawbacks of traditional luminescent materials, so that it can be applied in a wider range. In addition, the conversion of nano-materials, the side effects of small, for the biological tracer research is very helpful to solve the traditional material problems of security problems. In summary, the study of the upconversion material needs to be further, the synthesis method and the synthesis conditions are more perfect, can achieve large-scale reproduction of the production, so that the scope of its use to broaden.

In this paper, the upconversion luminescent material doped with rare earth ions was prepared by solvent method, and the oil-soluble material was changed outside, so as to increase the water solubility. The method was cyclodextrin coating method and mesoporous SiO2 coating. The synthesized nanoparticles were analyzed by fluorescence analysis, and the relevant information was obtained, which was prepared for further study.

Key Words: Rare-earth ion; Up-conversion; Solvent method; Surface modification

目 录

摘 要 I

Abstract II

第一章 前言 1

1.1荧光探针技术 1

1.2上转换纳米技术 2

1.2.1上转换的作用机理 2

1.2.2纳米荧光探针的优点 3

1.3稀土离子结构 4

1.3.1稀土的电子层结构 4

1.3.2 f-d电子跃迁 4

1.3.3电荷迁移带（Charge Transfer State, CTS）跃迁 4

1.3.4 f-d电子跃迁与CTS跃迁的区别 4

1.4主要合成方法 5

1.4.1水热法 5

1.4.2共沉淀法 5

1.4.3微乳液法 6

1.4.4高温热解法 6

1.5上转换发光材料的改性 6

1.5.1配体交换法 6

1.5.2 SiO₂包覆法 7

1.5.3配体氧化法 7

1.5.4聚合物包覆法 7

1.6稀土上转换纳米材料的应用 7

1.6.1生物成像 7

1.6.2生物检测 8

1.6.3生物芯片 8

1.7本论文研究内容和方法 8

第二章 实验部分 10

2.1实验药品试剂 10

2.2实验仪器设备 10

2.3实验步骤 10

2.3.1实验主要步骤 10

2.3.2合成纳米粒子 11

2.3.2.1根据改良方法合成OA-UCNP 11

2.3.2.2合成CD-UCNP 11

2.3.2.3包覆SiO₂ 11

第三章 结果与讨论 12

3.1 OA-UCNP的合成条件 12

3.2 CD-UCNP的合成条件 13

3.3谱图分析 13

3.3.1所得产物的荧光谱图和文献的荧光谱图的对比 13

3.3.2 NaYF₄: Er,Tm,Yb@SiO₂/CD的合成以及纳米粒子包裹前后的表征 14

3.3.3 XRD谱图的表征 15

3.3.4 TEM谱图的表征 16

第四章 结论与展望 17

参考文献 18

致 谢 21

1. 前言

1.1荧光探针技术

生物探针，是一类用来标记生物大分子（如蛋白质、核酸等）的示踪物质，通过化学键或吸附的方式与相关生物大分子结合，借助于荧光、化学发光、放射显影等方式来查看被标记物的有无或者其位置。

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