稀土氟化物纳米发光材料的制备及性能研究
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摘要
由于稀土离子独特的电子层结构,使得稀土发光材料具有优异的发光性能及广阔的应用前景。氟化物因其多样性的结构特点和特殊的物理化学特性,成为发光材料优良的基质。纳米级稀土发光材料的性质在很大程度上取决于其结构、形貌以及尺寸,因而合成出形貌和尺寸可控的纳米发光材料,成为科学工作者研究的热点。由于氨基酸具有特殊的官能团和自组装功能,因而能够用作模板来制备各种形态的纳米材料。
本论文采用精氨酸及其他表面活性剂辅助水热法制备出不同形貌的稀土氟化物纳米发光材料,对其结构和性能进行了表征。主要研究内容归纳如下:
1、以PEG-2000,柠檬酸和甘氨酸为表面活性剂,采用水热法制备出扁平纳米棒、纳米花和纳米片状GdF_3:Eu~(3+)发光材料,结果表明,表面活性剂种类,反应物浓度对产物的形貌均有影响;不同形貌样品的荧光光谱强度不同。以柠檬酸作表面活性剂,制备出梭状GdF_3:Yb~(3+),Er~(3+)纳米上转换发光材料,用980nm的激光激发,在上转换光谱图中可观察到绿色发射带和红色发射带。
2、采用精氨酸辅助水热法合成出空心“毛线团”状YF_3:Eu~(3+)纳米晶,讨论了反应时间与反应温度对形貌的影响,随着反应时间和反应温度的增加,产物形貌由实心球变为空心球。热处理后发光强度明显增强,Eu~(3+)掺杂YF_3纳米晶的发光强度随Eu~(3+)掺杂量的增加而增加,在10%时达到最大。并用此法制备了纳米YF_3:Yb~(3+),Er~(3+)上转换发光材料,并发射出很强的绿光、较强的红光及较弱的蓝光。
Rare earth luminescence materials have outstanding luminescent properties and wide potential application due to rare earth ions have special electronic shell structures. Fluorides become excellent host materials for luminescence materials owing to their diversity structural features,special physical and chemical characteristic. The properties of rare earth luminescent nano-materials largely depend on their structure, morphology and size.Therefore,the synthesis of luminescent nano-materials with controlled morphology and size has also aroused a lot of concern from the scientists. Amino acids can be used as templates to prepare nanomaterials with various shapes for their special functional group and self-assembling functions.
In this thesis, rare earth fluoride luminescence nano-materials with different morphologies were synthesized with arginine and other surfactant-assisted hydro-thermal method. The structure and properties were characterized. The results were summarized as follows:
1. GdF_3:Eu~(3+) nanomaterials with the morphologies of flat nanorods、nanoflowers and nanoflakes were prepared by PEG-2000,citric acid and glycine as surfactant-assisted hydrothermal method. Results showed that the morphologies are varied from the kinds of surfactants and the concentration of the reactant. The emission intensities are different from samples with different shapes. GdF_3:Yb~(3+),Er~(3+) upconversion luminescence nano-materials was prepared by citric acid-assisted hydrothermal method. Using 980nm laser as an exciting light, it can be observed the green emission band and red emission band in the upconversion fluorescenct spectra.
2. YF_3:Eu~(3+) hollow caddice spherelike were prepared by arginine-assisted hydrothermal method. The influences of reaction time and temperature on shapes were discussed. With the increase of reaction time and temperature, the shapes of the samples have been changed from solid spheres into hollow spheres. The luminescence intensity clearly enhanced after heat treatment. The luminescence intensity of the Eu~(3+)-doped YF_3 nanocrystal increased with the increasing doping concentration of Eu~(3+) ions and reached a maximum at 10mol%. YF_3:Yb~(3+),Er~(3+) shuttle-like upconversion luminescence nano-materials were prepared by the same method, the nano-crystals emitted the most bright green light, more intense red light and weaker blue light.
本论文采用精氨酸及其他表面活性剂辅助水热法制备出不同形貌的稀土氟化物纳米发光材料,对其结构和性能进行了表征。主要研究内容归纳如下:
1、以PEG-2000,柠檬酸和甘氨酸为表面活性剂,采用水热法制备出扁平纳米棒、纳米花和纳米片状GdF_3:Eu~(3+)发光材料,结果表明,表面活性剂种类,反应物浓度对产物的形貌均有影响;不同形貌样品的荧光光谱强度不同。以柠檬酸作表面活性剂,制备出梭状GdF_3:Yb~(3+),Er~(3+)纳米上转换发光材料,用980nm的激光激发,在上转换光谱图中可观察到绿色发射带和红色发射带。
2、采用精氨酸辅助水热法合成出空心“毛线团”状YF_3:Eu~(3+)纳米晶,讨论了反应时间与反应温度对形貌的影响,随着反应时间和反应温度的增加,产物形貌由实心球变为空心球。热处理后发光强度明显增强,Eu~(3+)掺杂YF_3纳米晶的发光强度随Eu~(3+)掺杂量的增加而增加,在10%时达到最大。并用此法制备了纳米YF_3:Yb~(3+),Er~(3+)上转换发光材料,并发射出很强的绿光、较强的红光及较弱的蓝光。
Rare earth luminescence materials have outstanding luminescent properties and wide potential application due to rare earth ions have special electronic shell structures. Fluorides become excellent host materials for luminescence materials owing to their diversity structural features,special physical and chemical characteristic. The properties of rare earth luminescent nano-materials largely depend on their structure, morphology and size.Therefore,the synthesis of luminescent nano-materials with controlled morphology and size has also aroused a lot of concern from the scientists. Amino acids can be used as templates to prepare nanomaterials with various shapes for their special functional group and self-assembling functions.
In this thesis, rare earth fluoride luminescence nano-materials with different morphologies were synthesized with arginine and other surfactant-assisted hydro-thermal method. The structure and properties were characterized. The results were summarized as follows:
1. GdF_3:Eu~(3+) nanomaterials with the morphologies of flat nanorods、nanoflowers and nanoflakes were prepared by PEG-2000,citric acid and glycine as surfactant-assisted hydrothermal method. Results showed that the morphologies are varied from the kinds of surfactants and the concentration of the reactant. The emission intensities are different from samples with different shapes. GdF_3:Yb~(3+),Er~(3+) upconversion luminescence nano-materials was prepared by citric acid-assisted hydrothermal method. Using 980nm laser as an exciting light, it can be observed the green emission band and red emission band in the upconversion fluorescenct spectra.
2. YF_3:Eu~(3+) hollow caddice spherelike were prepared by arginine-assisted hydrothermal method. The influences of reaction time and temperature on shapes were discussed. With the increase of reaction time and temperature, the shapes of the samples have been changed from solid spheres into hollow spheres. The luminescence intensity clearly enhanced after heat treatment. The luminescence intensity of the Eu~(3+)-doped YF_3 nanocrystal increased with the increasing doping concentration of Eu~(3+) ions and reached a maximum at 10mol%. YF_3:Yb~(3+),Er~(3+) shuttle-like upconversion luminescence nano-materials were prepared by the same method, the nano-crystals emitted the most bright green light, more intense red light and weaker blue light.
引文
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