稀土掺杂NaYF_4上转换纳米材料的制备、复合及物性研究
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摘要
稀土掺杂上转换纳米材料由于其独特的物理化学性质在生物标记、生物成像、光动力学治疗及药物输送等方面发挥了重要作用。本论文围绕稀土掺杂NaYF_4上转换纳米材料，建立了发光性能强、尺寸均匀、形貌可控的上转换纳米材料的制备方法，研究了反应参数对纳米材料形成的影响规律。为拓展纳米材料的功能性，采用简单实验方法设计合成了多种NaYF_4基功能性纳米复合材料，并对其结构、形貌及性质展开了系列研究工作，主要内容如下：
（1）对现有实验方法进行了优化，制备了尺寸、形貌、结构可控的NaYF_4: Yb~(3+),Er~(3+)上转换纳米材料，并研究各反应参数对其形成机制的影响。结果表明：溶剂热反应中调节稀土离子掺杂比例、表面活性剂含量、反应物比例及反应时间不仅可以得到不同颜色的发光、控制纳米材料的尺寸、还可实现纳米粒子从立方相向六方相的结构转变，从而增强上转换纳米材料的发光效率。实验选取发光效率较高的绿光发射NaYF_4:Yb~(3+), Er~(3+)上转换纳米材料，成功实现了对小白鼠体内不同位置的活体成像。
（2）为增强上转换纳米材料的水溶性及生物相容性，本文探索制备了NaYF_4: Yb~(3+),Er~(3+)/SiO_2核壳纳米复合材料并对其上转换发光性质进行分析。结果表明，反应中TEOS含量、反应时间、及反应浓度的增加易于导致SiO_2纳米粒子的自成核和纳米材料的交联。NaYF_4: Yb~(3+), Er~(3+)/SiO_2纳米复合材料的表面/界面对纳米材料的上转换发光性质产生一定影响。
（3）为进一步优化上转换纳米材料的发光性能，拓展其应用领域，本文利用静电纺丝方法将上转换纳米材料与有机高分子PVP相结合，通过调节纺丝电压和高温煅烧处理，制备了不同直径的NaYF_4:Yb~(3+), Er~(3+)/PVP和NaYF_4: Yb~(3+), Er~(3+)/SiO_2管状纳米复合材料，并对复合材料的形貌、结构及发光性能进行了研究。结果表明，通过改变纺丝电压，可以控制纳米管内径和外径的尺寸；PVP高分子能够有效的钝化上转换材料NaYF_4:Yb~(3+)Er~(3+)的表面缺陷，减少纳米材料无辐射跃迁几率，优化上转换发光性能。在此基础上，纳米复合材料经高温煅烧处理后，其红光发射得到了进一步的增强，这有利于提高材料在生物组织内的穿透深度，提高成像灵敏度。这类管状上转换纳米复合材料有望在药物缓释及其实时动态成像方面发挥潜在的应用价值。
（4）为拓展上转换纳米材料的功能性，本文将Fe_3O_4纳米粒子引入到NaYF_4: Yb~(3+)Er~(3+)纳米材料体系中，制备了Fe_3O_4/NaYF_4: Yb, Er磁光纳米复合材料。通过对复合材料物化性能的全面表征发现，这种Fe_3O_4/NaYF_4:Yb~(3+), Er~(3+)纳米复合材料同时具有NaYF_4:Yb~(3+), Er~(3+)组分的上转换发光性质和Fe_3O_4组分的超顺磁特性，这些优异的性质使这种磁光复合的纳米材料在生物分离、生物成像、生物检测及药物靶向运输等领域具有潜在的应用价值。
Rare earth ion doped up-conversion (UC) luminescent nanomaterials have been widelyapplied in biolabeling, bioimaging, photodynamic therapy and drug delivery due to theirunique physical and chemical properties. The present dissertation established thepreparation method of rare earth ion doped NaYF4UC nanomaterials with strongluminescence, uniform size and controlled morphology, and studied the effect of reactionparameters on the formation mechanism of the nanomaterials. To expand the functionality,we synthesized various NaYF4based multifunctional nanocomposite materials with simpleexperimental method, and carried out a series of investigations into the structure,morphology, and properties. The details are as following:
(1)The preparation methods were optimized. NaYF_4: Yb~(3+), Er~(3+)UC luminescencenanoparticles were prepared with controlled size, morphology and structure. The effect ofvarious reaction parameters on formation mechanism of the nanoparticles was analyzed.The experimental results showed that the size, phase structure, and luminescence propertiesof the UC luminescent nanoparticles can be controlled by adjusting various parameters,such as reaction time, the ratio of reactants, and the molar ratio of the rare earth ion. In vivoimaging of mice from different positions was achieved using NaYF_4: Yb~(3+), Er~(3+)UCluminescent nanoparticles with relatively high green emission.
(2)To enhance the water-solubility and biocompatibility of the UC luminescentnanomaterials, NaYF_4: Yb~(3+), Er~(3+)/SiO2core-shell nanocomposites were synthesized andtheir UC luminescence properties were analyzed. The results showed that the increase ofTEOS content, reaction time and concentration would lead to the self-nucleation of SiO2nanoparticles and cross-linking of nanoparticles. The surface/interface have an impact onUC luminescence properties of the nanocomposites.
(3) In order to further optimize the luminescent properties of UC nanomaterials andexpand their application areas, NaYF4: Yb~(3+), Er~(3+)/PVP and NaYF_4: Yb~(3+), Er~(3+)/SiO2nanotubes with various diameters were synthesized via electrospinning and hightemperature calcination. The inner and outer diameters of the nanotubes can be controlledby changing the electrospinning voltage. PVP molecules might produce the passivation onthe surface defects of NaYF_4: Yb~(3+), Er~(3+)nanoparticles and reduce the nonradiativerelaxation of Er~(3+)ion. After high temperature calcination, the red emissions of thenanotubes were further enhanced, which will facilitate to improve the penetration depth inbiotissues and enhance the sensitivity of imaging. The luminescent nanotubes with desirableUC properties are expected to have potential applications in drug delivery and real-timeimaging.
(4) To expand the functionality of the UC luminescent nanomaterials, thewater-soluble and surface-functionalized Fe_3O_4/NaYF4:Yb~(3+), Er~(3+)nanocubes were prepared.The results of magnetization curves and photoluminescence spectra revealed that thenanocubes simultaneously possessed the superparamagnetic properties of Fe_3O_4and UCluminescent properties of NaYF4: Yb~(3+), Er~(3+). These unique properties make thesemagnetic-upconversion nanomaterials promising candidates for bioseparation, bioimaging,biodetection, and targeted drug delivery.
（1）对现有实验方法进行了优化，制备了尺寸、形貌、结构可控的NaYF_4: Yb~(3+),Er~(3+)上转换纳米材料，并研究各反应参数对其形成机制的影响。结果表明：溶剂热反应中调节稀土离子掺杂比例、表面活性剂含量、反应物比例及反应时间不仅可以得到不同颜色的发光、控制纳米材料的尺寸、还可实现纳米粒子从立方相向六方相的结构转变，从而增强上转换纳米材料的发光效率。实验选取发光效率较高的绿光发射NaYF_4:Yb~(3+), Er~(3+)上转换纳米材料，成功实现了对小白鼠体内不同位置的活体成像。
（2）为增强上转换纳米材料的水溶性及生物相容性，本文探索制备了NaYF_4: Yb~(3+),Er~(3+)/SiO_2核壳纳米复合材料并对其上转换发光性质进行分析。结果表明，反应中TEOS含量、反应时间、及反应浓度的增加易于导致SiO_2纳米粒子的自成核和纳米材料的交联。NaYF_4: Yb~(3+), Er~(3+)/SiO_2纳米复合材料的表面/界面对纳米材料的上转换发光性质产生一定影响。
（3）为进一步优化上转换纳米材料的发光性能，拓展其应用领域，本文利用静电纺丝方法将上转换纳米材料与有机高分子PVP相结合，通过调节纺丝电压和高温煅烧处理，制备了不同直径的NaYF_4:Yb~(3+), Er~(3+)/PVP和NaYF_4: Yb~(3+), Er~(3+)/SiO_2管状纳米复合材料，并对复合材料的形貌、结构及发光性能进行了研究。结果表明，通过改变纺丝电压，可以控制纳米管内径和外径的尺寸；PVP高分子能够有效的钝化上转换材料NaYF_4:Yb~(3+)Er~(3+)的表面缺陷，减少纳米材料无辐射跃迁几率，优化上转换发光性能。在此基础上，纳米复合材料经高温煅烧处理后，其红光发射得到了进一步的增强，这有利于提高材料在生物组织内的穿透深度，提高成像灵敏度。这类管状上转换纳米复合材料有望在药物缓释及其实时动态成像方面发挥潜在的应用价值。
（4）为拓展上转换纳米材料的功能性，本文将Fe_3O_4纳米粒子引入到NaYF_4: Yb~(3+)Er~(3+)纳米材料体系中，制备了Fe_3O_4/NaYF_4: Yb, Er磁光纳米复合材料。通过对复合材料物化性能的全面表征发现，这种Fe_3O_4/NaYF_4:Yb~(3+), Er~(3+)纳米复合材料同时具有NaYF_4:Yb~(3+), Er~(3+)组分的上转换发光性质和Fe_3O_4组分的超顺磁特性，这些优异的性质使这种磁光复合的纳米材料在生物分离、生物成像、生物检测及药物靶向运输等领域具有潜在的应用价值。
Rare earth ion doped up-conversion (UC) luminescent nanomaterials have been widelyapplied in biolabeling, bioimaging, photodynamic therapy and drug delivery due to theirunique physical and chemical properties. The present dissertation established thepreparation method of rare earth ion doped NaYF4UC nanomaterials with strongluminescence, uniform size and controlled morphology, and studied the effect of reactionparameters on the formation mechanism of the nanomaterials. To expand the functionality,we synthesized various NaYF4based multifunctional nanocomposite materials with simpleexperimental method, and carried out a series of investigations into the structure,morphology, and properties. The details are as following:
(1)The preparation methods were optimized. NaYF_4: Yb~(3+), Er~(3+)UC luminescencenanoparticles were prepared with controlled size, morphology and structure. The effect ofvarious reaction parameters on formation mechanism of the nanoparticles was analyzed.The experimental results showed that the size, phase structure, and luminescence propertiesof the UC luminescent nanoparticles can be controlled by adjusting various parameters,such as reaction time, the ratio of reactants, and the molar ratio of the rare earth ion. In vivoimaging of mice from different positions was achieved using NaYF_4: Yb~(3+), Er~(3+)UCluminescent nanoparticles with relatively high green emission.
(2)To enhance the water-solubility and biocompatibility of the UC luminescentnanomaterials, NaYF_4: Yb~(3+), Er~(3+)/SiO2core-shell nanocomposites were synthesized andtheir UC luminescence properties were analyzed. The results showed that the increase ofTEOS content, reaction time and concentration would lead to the self-nucleation of SiO2nanoparticles and cross-linking of nanoparticles. The surface/interface have an impact onUC luminescence properties of the nanocomposites.
(3) In order to further optimize the luminescent properties of UC nanomaterials andexpand their application areas, NaYF4: Yb~(3+), Er~(3+)/PVP and NaYF_4: Yb~(3+), Er~(3+)/SiO2nanotubes with various diameters were synthesized via electrospinning and hightemperature calcination. The inner and outer diameters of the nanotubes can be controlledby changing the electrospinning voltage. PVP molecules might produce the passivation onthe surface defects of NaYF_4: Yb~(3+), Er~(3+)nanoparticles and reduce the nonradiativerelaxation of Er~(3+)ion. After high temperature calcination, the red emissions of thenanotubes were further enhanced, which will facilitate to improve the penetration depth inbiotissues and enhance the sensitivity of imaging. The luminescent nanotubes with desirableUC properties are expected to have potential applications in drug delivery and real-timeimaging.
(4) To expand the functionality of the UC luminescent nanomaterials, thewater-soluble and surface-functionalized Fe_3O_4/NaYF4:Yb~(3+), Er~(3+)nanocubes were prepared.The results of magnetization curves and photoluminescence spectra revealed that thenanocubes simultaneously possessed the superparamagnetic properties of Fe_3O_4and UCluminescent properties of NaYF4: Yb~(3+), Er~(3+). These unique properties make thesemagnetic-upconversion nanomaterials promising candidates for bioseparation, bioimaging,biodetection, and targeted drug delivery.
引文
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