CN116063330B - 高量子产率的稀土荧光材料及其制备方法 - Google Patents
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Abstract
高量子产率的稀土荧光材料及其制备方法，涉及到荧光材料领域。用五氟苯甲酸和邻菲罗琳做配体，均为无色晶体。通过五氟苯甲酸和氯离子诱导，使得整个化合物具有较强的刚性，且结晶于极性空间群，提高了发光效率。两个化合物均采用简单的溶剂热合成方法，产率和纯度较高。本发明中，在室温下，[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]在紫外线的激发下发射出明亮的红色和绿色荧光，量子产率分别为97.7％和90.7％。两个化合物表现出良好的热稳定性。该材料制备技术简单，设备要求不高，成本低廉，可望在防伪、生物体内成像以及LED等高新技术领域中得到广泛应用。
Description
技术领域
本发明涉及荧光材料领域，尤其涉及高量子产率的铕和铽稀土荧光材料及其制备方法。
背景技术
稀土荧光材料因其在化学传感、生物成像、生物探针、防伪、光信息传递和发光二极管等领域得到应用而受到广泛关注。稀土离子具有独特的电子结构和性质，但4f电子的禁阻跃迁限制了稀土离子的发光，导致稀土离子在发光强度、发光寿命和量子产率较差。关于发光性质的调控，可以通过加入化学物质来实现发光的变化。稀土与有机配体结合后能够发出高强度的纯正荧光，因此稀土有机配合物的合成与表征一直受到人们的普遍关注，为了探索新的发光材料，分析发光机理，人们利用不同的稀土离子与不同配体结合获得多种发光配合物用于研究其性能和应用。人们也尝试去探索降低配合物对称性来增强发光性质。但这些化合物基本存在着热稳定性差、合成复杂、量子产率低等方面的缺点，从而限制了应用。所以，寻找合成方法简便且高产率高性能的稀土发光配合物具有重要意义。
由于单一稀土离子发光效率低，稀土与合适的配体构成稀土配合物，配体吸收光能后将能量传递给稀土离子而发射强烈的稀土离子的特征荧光，但同时要注意稀土离子的配位数较高，水分子和溶剂分子容易参与配位，成为辐射能量的耗散通道。因此寻找合适的主配体与辅配体以及构筑刚性结构和低对称性稀土配合物，是人们努力的方向。
发明内容
本发明的目的在于解决现有技术中的上述问题，提供高量子产率的稀土荧光材料及其制备方法，制备具有纯度高、量子产率高、产率高、热稳定性好的高性能稀土荧光材料。
为达到上述目的，本发明采用如下技术方案：
本发明合成的荧光材料的化学式为[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]，均为正交晶系，其中铕化合物和铽化合物均结晶于Cmc21空间群，二者均为极性空间群。铕化合物单胞参数为α＝90°，β＝90°，γ＝90°，/>铽化合物单胞参数为/>α＝90°，β＝90°，γ＝90°，/>该材料具有刚性结构，在自然光下是白色的，热重分析表明热稳定性在250℃。室温下，[Eu1(Pfbza)2(Phen)1Cl]在紫外线的激发下发射出明亮的红色荧光，量子产率达97.7％，荧光寿命为1.7ms；[Tb1(Pfbza)2(Phen)1Cl]在紫外线的激发下发射出明亮的绿色荧光，量子产率为90.7％，荧光寿命为1.5ms。
本发明采用简单溶剂热法合成[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]荧光材料，具体过程如下：将五氟苯甲酸和邻菲罗琳溶解在乙醇中，向其中加入EuCl3或TbCl3，将所得的混合物装到玻璃瓶中，85℃溶剂热条件下保温3天，反应完后，冷却至室温，洗涤，干燥。
相对于现有技术，本发明技术方案取得的有益效果是：
本发明的[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]荧光材料，通过简单控制制备条件来获得高产率及高量子产率的纯相晶体，在紫外光下分别发出明亮的红色和绿色荧光。制备技术简单方便、设备要求不高、成本低廉，由于样品为晶体状态，且产率和纯度高，热稳定性好，可望在防伪、生物成像及LED等技术领域得到广泛应用。
附图说明
图1为[Eu1(Pfbza)2(Phen)1Cl]在室温下的固体荧光发射谱。
图2为[Tb1(Pfbza)2(Phen)1Cl]在室温下的固体荧光发射谱。
图3为[Eu1(Pfbza)2(Phen)1Cl]的热重图。
图4为[Tb1(Pfbza)2(Phen)1Cl]的热重图。
图5为[Eu1(Pfbza)2(Phen)1Cl]经不同温度处理后的粉末衍射谱图。
图6为[Tb1(Pfbza)2(Phen)1Cl]经不同温度处理后的粉末衍射谱图。
图7为[Eu1(Pfbza)2(Phen)1Cl]在室温下的寿命衰减图。
图8为[Tb1(Pfbza)2(Phen)1Cl]在室温下的寿命衰减图。
图9为[Eu1(Pfbza)2(Phen)1Cl]在室温下的量子产率实验数据图。
图10为[Tb1(Pfbza)2(Phen)1Cl]在室温下的量子产率实验数据图。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚、明白，以下结合附图和实施例，对本发明做进一步详细说明。
实施例1
将52.3mg(0.25mmol)的五氟苯甲酸、19.8mg(0.1mmol)的邻菲罗琳溶解在3mL的乙醇中，向溶液中加入36.6mg(0.1mmol)的EuCl3，将得到的混合物转入到4mL玻璃瓶中，盖紧盖子，放到85℃烘箱中，保温72小时。反应后，玻璃瓶随烘箱以2℃/秒的降温速度冷却到室温。结束后，过滤得到产物，用少量乙醇清洗，在真空干燥箱中放置24小时，得到洁净的无色[Eu1(Pfbza)2(Phen)1Cl]块状晶体，产率约为75.3％。元素分析理论值为(Eu1C26H8O4F10N2Cl1)：C 39.54，H 1.02，N 3.55；实验值为：C 39.32，H 1.07，N 3.54。红外谱吸收峰(KBr,cm-1)：746(s),850(m),930(w),995(s),1110(m),1401(m),1494(m),1611(m),1671(m).
实施例2
铽配合物的合成方法和铕配合物一样，只是将36.6mg(0.1mmol)的EuCl3换成37.3mg(0.1mmol)TbCl3。元素分析理论值为(Tb1C26H8O4F10N2Cl1)：C 39.19，H 1.01，N 3.52；实验值为:C 39.25，H 1.00，N 3.55。红外谱吸收峰(KBr,cm-1)：745(s),849(m),930(w),996(s),1110(m),1402(m),1490(m),1615(m),1675(m)。
从图1中可以看出，[Eu1(Pfbza)2(Phen)1Cl]在紫外光的激发下，发出强烈的Eu3+的特征红光，最强发射峰位于612nm；从图2中可以看出，[Tb1(Pfbza)2(Phen)1Cl]在紫外光的激发下，发出强烈的Tb3+的特征绿光，最强发射峰位于544nm。参见图3～6，从图中可以得出，本发明合成的稀土荧光材料具有较好的稳定性。图7和图8分别为铕化合物和铽化合物的寿命衰减图，从图中可以看出，两个化合物的寿命分别为1.7ms和1.5ms，而且两个化合物的实验数据和模拟数据非常契合。图9和图10分别为铕化合物和铽化合物的荧光量子产率实验数据图。本测试是采用绝对量子产率来表征的，即在数学上表示为发射光子数和吸收光子数的比值。在测试过程中，需要用到积分球附件，积分球内表面涂层是高反射性材料聚四氟乙烯，样品表面各个方向的激发光或者是发射光经过积分球均匀化后从出射口出来，进入到单色器中最后被检测器检测到。两个化合物在测试时，激发波长均为343nm，发射波长根据各自的发射光谱来确定。先测试空腔(只有积分球)的散射和发射，再测试带有样品的积分球的散射和发射，然后根据定义(发射光子数和吸收光子数)选定数据，仪器给出绝对量子产率的数值。测试结果为铕化合物的绝对量子产率为97.7％，铽化合物的绝对量子产率为90.7％。
本发明利用五氟苯甲酸和邻菲罗琳做配体，其分子式为[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]，均为无色晶体。通过五氟苯甲酸和氯离子诱导，使得整个化合物具有较强的刚性，且结晶于极性空间群，提高了发光效率。两个化合物均采用简单的溶剂热合成方法，产率和纯度较高。本发明中，在室温下，[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]在紫外线的激发下发射出明亮的红色和绿色荧光，量子产率分别为97.7％和90.7％。两个化合物表现出良好的热稳定性。该材料制备技术简单，设备要求不高，成本低廉，可望在防伪、生物体内成像以及LED等高新技术领域中得到广泛应用。
Claims (3)
1.高量子产率的稀土荧光材料，其特征在于：所述稀土荧光材料为铕荧光材料和铽荧光材料，化学式分别为[Eu1(Pfbza)2(Phen)1Cl]和[Tb1(Pfbza)2(Phen)1Cl]，均为正交晶系，其中铕化合物和铽化合物均结晶于Cmc21空间群，二者均为极性空间群，铕化合物单胞参数为a=26.3001(5) Å，b=11.9729(2) Å，c=7.7882(2) Å，α=90°，β=90°，γ=90°，V=2452.41(9)Å 3；铽化合物单胞参数为a=26.2825(7) Å，b=11.9356(3) Å，c=7.7662(2) Å，α=90°，β=90°，γ=90°，V=2436.24(3) Å 3；其中，化学式中的Pfbza表示去质子化的五氟苯甲酸。
2.权利要求1所述的高量子产率的稀土荧光材料的制备方法，其特征在于：将五氟苯甲酸和邻菲罗琳溶解在乙醇中，加入EuCl3或TbCl3，将所得混合物装到玻璃瓶中，溶剂热条件下反应，反应结束后，洗涤，干燥。
3.如权利要求2所述的高量子产率的稀土荧光材料的制备方法，其特征在于：溶剂热条件的温度为85±5℃。
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| CN115286647A (zh) * | 2022-07-29 | 2022-11-04 | 江西师范大学 | 一种双核稀土簇晶态材料的制备方法及其应用 |
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