CN106279222B - 一种钇掺杂铽配合物稀土发光材料及其制备方法 - Google Patents
一种钇掺杂铽配合物稀土发光材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种钇掺杂铽配合物稀土发光材料及其制备方法,其结构简式为:{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n,其基本结构是由Tb3+和Y3+形成双核结构单元,再由双核结构单元形成一维的链状结构;以bptcH4配体制备钇掺杂的铽配合物,具有重现好、合成简单、操作方便和产率高等特点;该钇掺杂铽配合物与未掺杂用纯苦味酸铽所制得的配合物材料相比,不仅结构保持不变,且材料的物理性质保持一致;在室温下,钇金属掺杂铽的配合物的荧光依然表现为稀土铽金属离子的四个特征峰,并与未掺杂用纯苦味酸铽所制得配合物的荧光光谱一致。
Description
技术领域
本发明涉及稀土磁性材料领域,具体的说是一种钇掺杂铽配合物稀土发光材料及其制备方法。
背景技术
由于稀土配合物是由稀土金属离子与有机配体通过配位反应或控制组装而形成的,因此其不仅具有无机物一样稳定好及兼具有机物那样荧光量子效率高等优点,而且其制备简便、易于修饰、荧光性质优异(包括荧光寿命长、发射谱带窄、色纯度高和发射光谱范围覆盖可见和近红外光区等)。近几十年来,稀土配合物发光材料一直是近年来的热门研究领域之一。
稀土配合物中,配体受激发态后的单重态能够跳跃到激发三线态,再由激发三线态将能量传递给中心金属离子,使中心离子激发产生荧光。因此,稀土配合物发光既可利用配体的三线态能量,又可利用激发单线态能量,综合这两方面的因素,稀土配合物的内量子效率很高,理论发光效率接近100%。
有稀土离子和有机配体形成的配合物,其荧光主要是受激发配体通过无辐射分子内能量传递将受激能量传递给中心离子,从而使中心稀土离子发出特征荧光。稀土离子这种发光现象称为“稀土敏化发光”。
对稀土离子铽而言,因外部的5s,5p电子对4f的电子的屏蔽,从而使铽离子受配体场地影响较少,进一步是铽离子的f-f跃迁呈现尖锐的线状谱带,且其激发态有相对长的寿命从而能够具有相对长的荧光寿命,并在光谱上表现为铽原子特有的类原子光谱的锐线谱,在不同的基质和晶场强度下,发光谱线的位置变化很少。
近年来的研究表明,在稀土配合物中引入不同的金属离子(包括过渡金属离子和稀土金属离子),可对其自身的光物理性质产生调制作用,实现稀土配合物材料在光学器件领域及生化领域的应用提供了重要的理论依据。
发明内容
本发明的目的是提供一种以较为廉价的钇金属掺杂铽配合物稀土发光材料及其制备方法,在不改变材料功能性的前提下,通过廉价的钇金属使用,极大的节约昂贵稀土铽的使用。
为解决上述技术问题,本发明采用的技术方案为:
一种钇掺杂铽配合物稀土发光材料,其结构简式为:{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n,其基本结构是由Tb3+和Y3+形成双核结构单元,再由双核结构单元形成一维的链状结构;所述材料属于三斜晶系,空间群为Pī,晶胞参数为a = 9.2137(16) Ǻ,b =9.2250(16) Ǻ,c = 9.4079(17) Ǻ,α = 87.213(2)°,β = 86.207(2)°,γ = 85.607(2)°,v = 794.8(2) Ǻ3;其中bptcH为2 ,2’-二吡啶基-3,3’,6,6’-四羧酸阴离子配体,其结构式为: 。
一种如上所述的钇掺杂铽配合物稀土发光材料的制备方法,在水热条件下,将苦味酸铽、苦味酸钇和2,2’-二吡啶基-3,3’,6,6’-四羧酸配体加入水中混合均匀后密封在反应釜内,在反应釜中加热至140~150℃,保温72小时后,自然冷却至室温,得到块状黄色晶体,再经过洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物。
所述的苦味酸铽、苦味酸钇和2,2’-二吡啶基-3,3’,6,6’-四羧酸配体加入量分别为:25mL水中加入0.05~0.15mmol苦味酸铽、0.05~0.15mmol苦味酸钇和0.1~0.3mmol的2,2’-二吡啶基-3,3’,6,6’-四羧酸。
所述的苦味酸铽为11水合苦味酸铽。
所述的苦味酸钇为11水合苦味酸钇。
所述反应釜为内衬聚四氟乙烯的不锈钢高压反应釜。
本发明的有益效果:
本发明提供的钇掺杂铽配合物稀土发光材料的制备方法,以bptcH4配体制备钇掺杂的铽配合物,具有重现好、合成简单、操作方便和产率高等特点;该钇掺杂铽配合物与未掺杂用纯苦味酸铽所制得的配合物材料相比,不仅结构保持不变,且材料的物理性质保持一致;在室温下,钇金属掺杂铽的配合物的荧光依然表现为稀土铽金属离子的四个特征峰,并与未掺杂用纯苦味酸铽所制得配合物的荧光光谱一致。研究表明:在相同的条件下,以bptcH4配体制备钇掺杂的铽配合物的结构和发光性能与该配体制备的纯铽化合物的结构和发光性能非常相似,因此,本发明在不改变材料功能性的前提下,通过廉价的钇金属使用,极大的节约昂贵稀土铽的使用。
附图说明
图1为实例1制备的钇金属掺杂铽配合物配位图;
图2为实例1制备的钇金属掺杂铽配合物的一维链状结构;
图3为实例1制备的钇金属掺杂铽配合物与未掺杂铽配合物的荧光光谱。
具体实施方式
下面结合具体实施方式对本发明做进一步的阐述。
一种钇掺杂铽配合物稀土发光材料,其结构简式为:{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n,其基本结构是由Tb3+和Y3+形成双核结构单元,再由双核结构单元形成一维的链状结构;所述材料属于三斜晶系,空间群为Pī,晶胞参数为a = 9.2137(16) Ǻ,b =9.2250(16) Ǻ,c = 9.4079(17) Ǻ,α = 87.213(2)°,β = 86.207(2)°,γ = 85.607(2)°,v = 794.8(2) Ǻ3;其中bptcH为2 ,2’-二吡啶基-3,3’,6,6’-四羧酸阴离子配体,其结构式为:。
一种如上所述的钇掺杂铽配合物稀土发光材料的制备方法,在水热条件下,将苦味酸铽、苦味酸钇和2,2’-二吡啶基-3,3’,6,6’-四羧酸配体加入水中混合均匀后密封在反应釜内,在反应釜中加热至140~150℃,保温72小时后,自然冷却至室温,得到块状黄色晶体,再经过洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物;其中2 ,2’-二吡啶基-3,3’,6,6’-四羧酸配体(bptcH4)结构式为:
。
实施例1
将0.05 mmol苦味酸铽(52.1毫克)、0.05 mmol苦味酸钇(48.6毫克)和0.1 mmol2,2’-二吡啶基-3,3’,6,6’-四羧酸配体(33.2毫克)加入25 mL水中,混合均匀后密封在一个内衬聚四氟乙烯的不锈钢高压反应釜内,在高压反应釜中加热到140~150℃,保温72小时冷却至室温,得到块状黄色晶体,先经过少量DMF洗涤,再经过大量水洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物,产率为92%。
钇掺杂铽配合物表征其过程如下:
(1)钇掺杂铽配合物的单晶结构测定
选取质量较好和大小合适的晶体粘于一根玻璃丝上,置于Bruker SMART ApexII单晶衍射仪上进行单晶结构测定:23℃下,采用MoK a (λ= 0.71073 Å)射线作为光源,石墨作为单色器,检测面板为Bruker Smart CCD,用ω扫描方式对晶胞进行扫描测定并收集衍射强度数据。首先采用BrukerAPEXII 程序对采集好的数据进行晶胞精修、数据的吸收校准以及还原;然后通过 SHELXTL 软件中的XS 程序对还原后的数据采用直接法解析结构,获得所有非氢原子的初始相位角,各向异性参数的精修则通过SHELXL-97 程序运行,使用全矩阵最小二乘法,直至数据收敛,最终对非氢原子坐标的进行确定。芳香环上与碳原子相连的氢均通过理论计算法加入。水分子上的氢原子通过差值Fourier合成法得到并将其固定在氧原子上进行精修。详细的晶体测试参数见表一,重要的选择性键长和键角见表二。晶体的结构图见图1,图2。
表一 钇掺杂铽配合物的晶体学参数
表二 钇掺杂铽配合物的选择性键长和键角
对称操作:i x-1, y, z; ii -x+2, -y+1, -z+2; iii-x+1, -y+1, -z+2
(2)钇掺杂铽配合物的荧光测试
将所得的钇掺杂铽配合物在Hitachi/F-4500荧光测试仪上进行样品固体荧光测定,其谱图见图3所示。由图可知,在激发波长λ ex为340 nm,钇金属掺杂铽配合物的荧光表现为稀土铽金属离子的四个特征峰,分别为5D4→7FJ (J = 3, 4, 5, 6), 5D4→7F6 (491 nm)5D4→7F5 (546 nm), 5D4→7F4 (584 nm), 以及 5D4→7FJ (620 nm)。这与未掺杂用纯苦味酸铽所制得配合物的荧光光谱一致,只是峰强度稍微减弱。
(3)钇掺杂铽配合物的元素分析测试
钇掺杂铽配合物用意大利产的Flash EA-2000元素分析仪进行元素分析,测试表明C、N、H三元素的测定值与理论计算值相近,其测试结果数据如下:对分子式为C28H22Tb1.03N4O22Y0.97的钇掺杂铽配合物其理论值为:C 33.09, H 2.18, N 5.51; 实验测值:C 33.42, H 2.28, N 5.61.
实施例2
将0.1 mmol苦味酸铽(104.1毫克)、0.1 mmol苦味酸钇(97.1毫克)和0.2 mmol 2,2’-二吡啶基-3,3’,6,6’-四羧酸配体(66.4毫克)加入25 mL水中,混合均匀后密封在一个内衬聚四氟乙烯的不锈钢高压反应釜内,在高压反应釜中加热到140~150℃,保温72小时冷却至室温,得到块状黄色晶体,先经过少量DMF洗涤,再经过大量水洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物,产率为89%。
实施例3
将0.15mmol苦味酸铽(156.2毫克)、0.15mmol苦味酸钇(145.7毫克)和0.3 mmol2,2’-二吡啶基-3,3’,6,6’-四羧酸配体(99.7毫克)加入25 mL水中,混合均匀后密封在一个内衬聚四氟乙烯的不锈钢高压反应釜内,在高压反应釜中加热到140~150℃,保温72小时冷却至室温,得到块状黄色晶体,先经过少量DMF洗涤,再经过大量水洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物,产率为86%。
实施例4
将0.05 mmol苦味酸铽(52.1毫克)、0.05 mmol苦味酸钇(48.6毫克)和0.1 mmol2,2’-二吡啶基-3,3’,6,6’-四羧酸配体(33.2毫克)加入25 mL水中,混合均匀后密封在一个内衬聚四氟乙烯的不锈钢高压反应釜内,在高压反应釜中加热到140~145℃,保温72小时冷却至室温,得到块状黄色晶体,先经过少量DMF洗涤,再经过大量水洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物,产率为89%。
实施例5
将0.05 mmol苦味酸铽(52.1毫克)、0.05 mmol苦味酸钇(48.6毫克)和0.1 mmol2,2’-二吡啶基-3,3’,6,6’-四羧酸配体(33.2毫克)加入25 mL水中,混合均匀后密封在一个内衬聚四氟乙烯的不锈钢高压反应釜内,在高压反应釜中加热到145~150℃,保温72小时冷却至室温,得到块状黄色晶体,先经过少量DMF洗涤,再经过大量水洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)(H2O)2]·H2O}n的钇掺杂铽配合物,产率为89%。
Claims (3)
1.一种钇掺杂铽配合物稀土发光材料的制备方法,所述钇掺杂铽配合物稀土发光材料的结构简式为:{[Tb1.07Y0.93(bptcH)2 ( H2O)4] ·2H2O}n,其基本结构是由Tb3+和Y3+形成双核结构单元,再由双核结构单元形成一维的链状结构;所述材料属于三斜晶系,空间群为Pī,晶胞参数为a = 9.2137(16) Å ,b = 9.2250(16) Å ,c = 9.4079(17) Å ,α = 87.213(2)°,β = 86.207(2)°,γ = 85.607(2)°,v = 794.8(2) Å3 ;其中bptcH为2 ,2’-二吡啶基-3,3’,6,6’-四羧酸阴离子配体,其结构式为:;
其特征在于:在水热条件下,将苦味酸铽、苦味酸钇和2,2’-二吡啶基-3,3’,6,6’-四羧酸配体加入水中混合均匀后密封在反应釜内,在反应釜中加热至140~150℃,保温72小时后,自然冷却至室温,得到块状黄色晶体,再经过洗涤和干燥,得到结构式为{[Tb1.07Y0.93(bptcH)2 ( H2O)4] ·2H2O}n的钇掺杂铽配合物。
2.如权利要求1所述的钇掺杂铽配合物稀土发光材料的制备方法,其特征在于:所述的苦味酸铽、苦味酸钇和2,2’-二吡啶基-3,3’,6,6’-四羧酸配体加入量分别为:25mL水中加入0.05~0.15mmol苦味酸铽、0.05~0.15mmol苦味酸钇和0.1~0.3mmol的2,2’-二吡啶基-3,3’,6,6’-四羧酸。
3.如权利要求1所述的钇掺杂铽配合物稀土发光材料的制备方法,其特征在于:所述反应釜为内衬聚四氟乙烯的不锈钢高压反应釜。
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"Syntheses, Structures, Luminescence, and Magnetic Properties of One-dimensional Lanthanide Coordination Polymers with a Rigid 2,2′-Bipyridine-3,3′,6,6′-tetracarboxylic Acid Ligand";Baoming Ji et al.;《Inorganic Chemistry》;20120202;第51卷;第2170-2177页 * |
"吡啶多羧酸配合物的合成、性质及新型双膦配体的合成研究";何晓;《万方数据-学位论文》;20100201;论文第17页配合物1-2,5,论文第22页表2-1,第31页表2-11,论文第59页图2-17 * |
"稀土有机发光材料制备及性能的研究";吕玉光;《万方数据-学位论文》;20110215;论文第3-4页 * |
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