稀土掺杂低维结构荧光粉的湿法合成与光热转换特性的研究

发布时间：2018-12-10 16:54

【摘要】：载运作为连接国民经济体系的桥梁,提高载运工具的节能环保能力有着重要现实意义。稀土掺杂的固态照明光源在汽车、船舶和飞机等载运工具上的运用,可大幅减少能源的消耗,提高这些载运工具的节能环保能力。同时稀土离子温度传感和光热转换特性有望在载运工具精密微电子仪器的监测和维护上具有潜在应用。纳米科学技术的发展赋予了低维纳米材料的新的光、电、磁、声和催化性能,实现低维纳米材料的可控合成具有重要意义,因此成为了当前的热门研究课题。此外,稀土掺杂的光热转换材料在船舶压载水的微生物灭活领域还存在着潜在应用。本文研究了稀土掺杂微纳米材料的湿法化学可控合成,并对这些稀土离子在低维纳米材料中的温度传感和光热转换特性进行了详细的研究,主要研究成果如下:(1)采用微波水热法成功地制备了 CaSn03、NaYF_4、YP04、NaLa(W04)2和NaLa(Mo04)2微纳结构材料,证明了微波水热合成在无机物体系合成中普适性,并对这些样品的晶体学和形貌学特征进行了表征和分析,结果证明所合成的样品大部分为纯相且其形貌受配合物和反应溶液pH值等因素的影响。(2)采用微波水热法制备了 NaY(WO_4)_2微米花球,样品的XRD表征结果证实所得产物为纯相NaY(WO_4)_2。样品SEM表征结果说明了配合物Na3Cit的用量对产物形貌的影响,据此推论出了 NaY(WO_4)_2微米花球的可能的生长机理。(3)实现了微波水热条件下NaY(MoO_4)_2多种微纳米结构的可控合成,研究了反应溶液pH值、配合物浓度、反应物浓度等因素对产物晶相和形貌的影响,给出了 NaY(WO_4)_2微纳米结构的可能的生长机理。(4)研究了Er~(3+)离子在NaY(WO_4)_2微米花球体系中的温度传感特性,揭示了样品形貌、Er~(3+)离子掺杂浓度和Yb~(3+)离子掺杂浓度对Er~(3+)离子温度传感特性的微弱影响。以Er~(3+)掺杂的NaY(WO4)2微米花球为荧光温度探针,研究了 Tm~(3+)掺杂NaY(WO_4)_2微米花球的光热转换特性,证明了 Tm~(3+)离子与Er~(3+)相比,Tm~(3+)离子具有更高的光热转换效率。(5)以Er~(3+)掺杂的NaY(MoO_4)_2纳米棒为荧光温度探针,研究了Sm~(3+)掺杂同基质材料的光热转换特性。结果证明,Sm~(3+)离子和Yb~(3+)离子的掺杂浓度都会对样品的光热转换特性产生影响,且Yb~(3+)离子的浓度影响更为显著。(6)采用高温热解法成功制备了 NaYF_4:Er~(3+)/Yb~(3+)@NaYF_4:Sm~(3+)/Yb~(3+)纳米核壳结构,XRD表征结果证明所合成的样品为纯相,且壳层包覆使样品的结晶度更好。TEM表征结果证明壳层Yb~(3+)掺杂离子浓度的变化对产物的最终尺寸和形貌有影响。实现了核层的温度传感和壳层的光热转换,且加热效果受壳层Yb~(3+)离子浓度的影响。
[Abstract]:As a bridge connecting the national economic system, it is of great practical significance to improve the energy saving and environmental protection ability of transportation tools. The application of rare-earth doped solid state lighting source in vehicles, ships and aircraft can greatly reduce the energy consumption and improve the energy saving and environmental protection ability of these vehicles. At the same time, the temperature sensing and photothermal conversion characteristics of rare earth ions are expected to have potential applications in monitoring and maintenance of precision microelectronic instruments. With the development of nanometer science and technology, the new optical, electrical, magnetic, acoustic and catalytic properties of low-dimensional nanomaterials have become a hot research topic. It is of great significance to realize the controllable synthesis of low-dimensional nanomaterials. In addition, rare earth doped photothermal conversion materials have potential applications in the field of microbial inactivation of ship ballast water. In this paper, the wet chemically controlled synthesis of rare earth doped micro and nano materials is studied, and the temperature sensing and photothermal conversion characteristics of these rare earth ions in low dimensional nanomaterials are studied in detail. The main results are as follows: (1) CaSn03,NaYF_4,YP04,NaLa (W04) 2 and NaLa (Mo04) 2 microstructures were successfully prepared by microwave hydrothermal method. The crystallographic and morphologic characteristics of these samples were characterized and analyzed. The results show that most of the synthesized samples are pure phase and their morphology is influenced by the complex and pH value of reaction solution. (2) NaY (WO_4) _ 2 micron flower spheres were prepared by microwave hydrothermal method. The XRD characterization of the sample confirmed that the product was pure phase NaY (WO_4) _ 2. The results of SEM characterization showed that the amount of complex Na3Cit affected the morphology of the product. The possible growth mechanism of NaY (WO_4) _ 2 microspheres was deduced. (3) the controllable synthesis of NaY (MoO_4) _ 2 microstructures under hydrothermal conditions was achieved, and the pH value of reaction solution and the concentration of complex were studied. The effect of reactant concentration on the crystal phase and morphology of the product, The possible growth mechanism of NaY (WO_4) _ 2 microstructures was given. (4) the temperature sensing properties of Er~ (3) ions in NaY (WO_4) _ 2 micron-sphere system were studied, and the morphology of the samples was revealed. The weak effect of Er~ (3) ion doping concentration and Yb~ (3) ion doping concentration on the temperature sensing characteristics of Er~ (3) ion. Using Er~ (3) doped NaY (WO4) 2 microsphere as the fluorescence temperature probe, the photothermal conversion characteristics of Tm~ (3) doped NaY (WO_4) 2 microsphere were studied. It was proved that the Tm~ (3) ion was compared with Er~ (3). Tm~ (3) ions have higher photothermal conversion efficiency. (5) Er~ (3) doped NaY (MoO_4) _ 2 nanorods were used as fluorescence probe to investigate the photothermal conversion properties of Sm~ (3) doped with the substrate. The results show that the doping concentration of Sm~ (3) and Yb~ (3) ions will affect the photothermal conversion characteristics of the samples. The effect of Yb~ (3) ion concentration was more significant. (6) NaYF_4:Er~ (3) / Yb~ (3) @ NaYF_4:Sm~ (3) / Yb~ (3) nanocrystalline core-shell structure was successfully prepared by high temperature pyrolysis. The results of XRD show that the synthesized samples are pure phase, and the crystallinity of the samples is improved by coating the shell layer. The results of TEM characterization show that the change of the concentration of Yb~ (3) doped ions in the shell layer has an effect on the final size and morphology of the product. The temperature sensing of the core layer and the photothermal conversion of the shell layer are realized, and the heating effect is affected by the concentration of Yb~ (3) ions in the shell layer.
【学位授予单位】：大连海事大学
【学位级别】：博士
【学位授予年份】：2017
【分类号】：U664.92

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