稀土掺杂复合氟化物纳米颗粒的合成及其上转换发光性质研究

发布时间：2018-03-21 20:50

  本文选题：稀土　切入点：上转换发光　出处：《内蒙古师范大学》2013年硕士论文　论文类型：学位论文

【摘要】：稀土发光材料是指利用稀土元素独特的电子层结构、采用不同激发方式而使其发光的稀土功能材料。目前，稀土发光材料在照明、显示、生物标签和数据储存等领域有着广泛的应用前景，也正向其他新兴技术领域扩展。 本文的主要研究目的是合成尺寸较小形貌规则的稀土掺杂复合氟化物纳米颗粒，使之应用于荧光成像和制造激光器件。我们采用水热法合成了形貌规则的β-Na(Y_(1.5-x-y)Na_(0.5))F_6: Yb_x~(3+), Tm_y~(3+)、LiYF_4:Yb_x~(3+), Tm_y~(3+)和β-NaGd_(0.794)Yb_(0.20)Ho_(0.001)Tm_(0.005)F_4纳米颗粒，并通过980nm二极管激光器（中国科学院北京半导体所）激发下，采用Hitachi F-4600荧光分光光度计测量了样品发射光谱。采用荷兰Philips公司生产的Pw1830型X-射线粉末衍射仪（XRD，，其X射线波长为λ=0.15406nm）对样品进行了物相分析。利用JEM2010型透射电子显微镜（TEM，其工作电压为200kV）和高分辨透射电子显微镜（HRTEM）观察产物的尺寸和形貌，利用电子能谱仪（EDS）分析样品的组成。 本论文的主要研究结果： (1)我们利用水热合成法制备了形貌规则的六角相β-Na(Y_(1.5-x-y)Na_(0.5))F_6:Yb_x~(3+),Tm_y~(3+)纳米颗粒。XRD和TEM分析结果显示纳米颗粒平均粒径约为22nm。不同掺杂浓度的敏化剂Yb~(3+)和激活剂Tm~(3+)的室温上转换发射光谱分析结果表明样品有紫外、蓝色和红色5个发射带，其辐射跃迁分别是Tm~(3+)的~1I_6→~3F_4、~1D_2→~3H_6、~1D_2→~3F_4、~G1_4→~3H_6和~1G_4→~3F_4，敏化剂和激活剂最佳掺杂浓度分别为60%和0.6%。(2)我们利用水热合成法制备了LiYF_4:Yb_x~(3+x),Tm_y~(3+)纳米颗粒。XRD和TEM分析结果显示纳米颗粒平均粒径约为36nm。不同掺杂浓度的敏化剂Yb~(3+)和激活剂Tm~(3+)的室温上转换发射光谱分析结果表明样品有紫外、蓝色和红色5个发射带，其辐射跃迁分别是Tm~(3+)的~1I_6→~3F_4、~1D_2→~3H_6、~1D_2→~3F_4、~1G_4→~3H_6和~1G_4→~3F_4，敏化剂和激活剂最佳掺杂浓度分别为60%和0.6%。此结果与合成β-Na(Y_(1.5-x-y)Na_(0.5)F_6:Yb_x~(3+),Tm_y~(3+)纳米颗粒的结果一致，表明第一族元素Na和Li作为基质复合氟化物的稀土Yb~(3+)，Tm~(3+)掺杂纳米材料的发光性质较相似。 (3)我们利用简单的水热法合成了β-NaGd_(0.794)Yb_(0.20)Ho_(0.001)Tm_(0.005)F_4纳米颗粒。XRD分析结果表明样品为六角物相。同时我们观察到了YbF3的两个X-射线衍射峰。TEM分析结果说明，样品具有椭球和六角两种形貌，其平均边长为23nm。室温上转换发射光谱分析结果告诉我们，样品是由Tm~(3+)离子的蓝色发光和Ho~(3+)离子的绿色、红色发光组成白色上转换发光。根据色品分析结果得知，白色光的色品坐标分别为CIE-X=0.2717和CIE-Y=0.2673。
[Abstract]:Rare earth luminescent material is a kind of rare earth functional material which uses the unique electronic layer structure of rare earth elements and uses different excitation ways to make it luminous. At present, rare earth luminescent materials are illuminated and displayed. Biolabelling and data storage have a wide range of applications and are expanding to other emerging technologies. The main purpose of this paper is to synthesize rare earth doped composite fluoride nanoparticles with small size and regular morphology. For use in fluorescent imaging and laser devices, we have hydrothermal synthesis of regular 尾 -NaGdtir 1.5-x-yn NaS-1. 5 / F6: Yb_x~(3: Yb_x~(3, Tm_y~(3 / LiYF4: YbxS, Tm_y~(3) and 尾 -NaGd0.794Ybb / 0.20HoGd0.20 Hob / 0.20 / 0.20 / 0. 001T / T / T / P / P / F4 nanoparticles, excited by a 980nm diode laser (Beijing Semiconductor Institute of the Chinese Academy of Sciences), and by means of a 980nm diode laser (Beijing Semiconductor Institute of the Chinese Academy of Sciences). The emission spectrum of the sample was measured by Hitachi F-4600 fluorescence spectrophotometer. The phase analysis of the sample was carried out by using the Pw1830 X-ray powder diffractometer made by Philips Company of the Netherlands, the X-ray wavelength of which was 位 0.15406nm. the JEM2010 transmission electron display was used to analyze the phase of the sample. The size and morphology of the products were observed by micromirror Tem with a working voltage of 200kV) and HRTEM with high resolution transmission electron microscopy (HRTEM). The composition of the sample was analyzed by electron energy spectrometer (EDS). The main results of this thesis are as follows:. (1) We have prepared hexagonal phase 尾 -NaANGYANGYX (1.5-x-YS) 0.5D, F6: YbxX ~ (3) T _ myY _ (3) by hydrothermal synthesis method. The results of TEM and XRD analysis show that the average particle size is about 22 nm. The sensitizer Yb~(3 with different doping concentration and the activator Tm~(3) have been prepared at room temperature. The results of the analysis are as follows: (1) the average particle size of the hexagonal phase is about 22 nm, and that of the activator Tm~(3) is different from that of the sensitizer (Yb~(3) with different doping concentration. The results of conversion emission spectrum analysis showed that the samples had UV, Blue and red emission bands with radiation transitions of Tm~(3). 鈫

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