铕、铽掺杂的下转换发光材料的制备及性能研究

Synthesis and Optical Properties of dowm-conversion Luminescent Materials Doped by Eu\Tb

作者: 专业:无机化学 导师:李中军 年度:2010 学位:硕士  院校: 郑州大学

Keywords

CaF2, Eu, Tb, doping, nanoparticles, luminous materials

        多年来,人们一直没有停止过对新型发光材料的开发和探索。稀土离子的独特电子结构,使稀土掺杂发光材料具有光化学稳定、荧光寿命长、量子产率高、发射光谱窄、Stokes位移大等独特优点。因此,镧系掺杂发光材料一直是人们研究的焦点。Eu3+、Tb3+分别是红色和绿色荧光粉中最常用最重要的激活剂,更是人们研究焦点中的焦点。本论文主要针对铕、铽掺杂的下转换发光材料的制备及水溶性开展一些工作,主要内容归纳如下:1.以甲醇作反应溶剂,采用共沉淀法,在不使用任何表面活性剂的情况下,制得了亲水性的CaF2:Ln3+纳米颗粒,这些颗粒能很好的分散在水中,且颗粒分布均匀,平均粒径在20nm左右,没有发生团聚现象。此方法操作简单、重现性好、产率高,非常适合大量生产。2.分别采用聚乙烯吡咯烷酮(PVP)和柠檬酸作为表面活性剂,用共沉淀法和水热法制得了亲水性的CaF2:Ln3+纳米颗粒,这些颗粒能很好的分散在水中,并详细研究了其结构及荧光性能。3.通常情况下球形的CaF2:Eu3+颗粒很难得到,本论文通过正硅酸乙酯的催化水解制得单分散的球形SiO2颗粒,然后在其它活性剂的作用下,在其表面包覆一层具有荧光性能的CaF2:Eu3+,这样即制得了一种球形发光材料,又节省了稀土元素。4.采用水热法合成了Eu3+和PO43-离子共掺杂的CaPxW1-xO4:Eu3+纳米材料,经XRD、TEM及荧光光谱分析表明,颗粒是典型的白钨矿结构;形貌呈棒状;PO43-离子的掺入可以有效的调节光谱强度,改变PO43-离子的掺杂浓度可得到不同发射强度的荧光材料。
    For years, scientists have not stopped the exploitation and exploration of new types of light-emitting materials. The unique electronic structure of tombarthite ions enables tombarthite mixed with light-emitting materials to have the qualities of possessing the stability of photochemistry, long life span of fluorescence, a high productivity of quantum, a narrow optical spectrum, a large Stokes shift etc. It has long been the focus of the study. Eu3+、Tb3+ separately are the most commonly used as the activator in red and green phosphors, which are for more the key points in this paper. This paper aims at the research, of luminous materials obtaining impured with Eu3+ and Tb3+ and their water-solubility, mainly summarized as follows:1. Using methanol as solvent, along with using co-precipitation method, to get the hydrophilic CaF2:Ln3+nanoparticles without using any surfactant. These particles can be well dispersed and distributed in water, and the average particle size is about 20nm, without agglomeration. This method is simple, reproducible, high yield, and very suitable for mass production.2. Separately by adopting PVP and citric acid as surfactants, plus co-precipitation method and hydrothermal process to get he hydrophilic CaF2:Ln3+nanoparticles. And these particles are well distibuted. We deeply study its structure and its fluorescence property.3. Generally spherical CaF2:Ln3+particles are difficult to obtain. By catalyzation and hydrolyzation of TEOS we can get the monodispersed spherical SiO2 particles, and then under the effect of other activator, we can coat its surface a layer with the fluorescence properties of CaF2:Eu3+. Doing this, we not only get a spherical luminescent material, but save the tombarthite elements and reduce costs.4. By using hydrothermal process we can synthesize CaPxW1-xO4:Eu3+ nano materials doped with Eu3+ and. Taking XRD and TEM and fluorescent optical spectrum into analysis, it reveals that granul it the typical rod-like scheelite structure. The combination of PO43- ions can effectively adjust the intensity of fluorescent optical spectrum. Varying the doping density of PO43- ions can get a different emitting intensity of fluorescent materials.
        

铕、铽掺杂的下转换发光材料的制备及性能研究

摘要4-5
abstract5-6
第一章 绪论10-25
    1.1 发光材料的定义和分类10-12
        1.1.1 光致发光10-11
        1.1.2 电致发光11
        1.1.3 x射线及高能粒子发光11
        1.1.4 阴极射线发光11
        1.1.5 化学发光11-12
    1.2 稀土发光材料12-15
        1.2.1 稀土离子的发光特性12-15
        1.2.2稀土发光材料的优点15
    1.3 稀土发光材料的制备方法15-17
        1.3.1 沉淀法16
        1.3.2 水热法16-17
        1.3.3 溶胶-凝胶法17
        1.3.4 微乳液法17
    1.4 稀土发光材料的表面改性与核-壳结构17-19
    1.5 本论文的选题思路和主要内容19-21
    参考文献21-25
第二章 亲水性CaF_2:Ln~(3+)纳米材料的制备及性能研究25-35
    2.1 引言25
    2.2 实验部分25-26
        2.2.1 试剂及仪器25-26
        2.2.2 纳米材料的制备方法26
    2.3 结果与讨论26-32
        2.3.1 样品的结构与形貌26-27
        2.3.2 纳米材料的红外分析27-28
        2.3.3 样品的发光性能28-32
    2.4 本章小结32-33
    参考文献33-35
第三章 有机配体修饰的亲水性CaF_2:Ln~(3+)复合材料的制备及性能研究35-47
    3.1 引言35
    3.2 实验部分35-37
        3.2.1 试剂与仪器35-36
        3.2.2 制备方法36-37
    3.3 PVP修饰的CaF_2:Ln~(3+)复合材料37-40
        3.3.1 样品的结构与形貌37-38
        3.3.2 样品的红外分析38-39
        3.3.3 样品的发光性能39-40
    3.4 柠檬酸修饰的CaF_2:Ln~(3+)复合材料40-44
        3.4.1 样品的结构与形貌40-41
        3.4.2 样品的红外分析41-42
        3.4.3 样品的发光性能42-44
    3.5 本章小结44-45
    参考文献45-47
第四章 SiO_2@CaF_2:Eu~(3+)核壳型发光材料的制备及性能研究47-54
    4.1 引言47
    4.2 实验部分47-48
        4.2.1 试剂及仪器47-48
        4.2.2 制备方法48
    4.3 结果与讨论48-52
        4.3.1 样品的结构与形貌48-51
        4.3.2 样品的发光性能51-52
        4.3.3 包覆次数对荧光性能的影响52
    4.4 本章小结52-53
    参考文献53-54
第五章 荧光可调的CaP_xW_(1-x)O_4:Eu~(3+)的制备及性能研究54-61
    5.1 引言54
    5.2 实验部分54-55
        5.2.1 试剂及仪器54-55
        5.2.2 制备方法55
    5.3 结果与讨论55-59
        5.3.1 样品的结构与形貌55-57
        5.3.2 样品的红外分析57
        5.3.3 样品的发光性能57-59
    5.4 本章小结59
    参考文献59-61
致谢61-62
个人简历及硕士期间发表论文62
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