CN108484647A - 一种钕配合物及其制备方法和应用 - Google Patents
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Abstract
本发明涉及一种钕配合物及其制备方法,配合物结构简式为:[Nd2(TCPB)2(DMF)(H2O)]n,其中H3TCPB为1,3,5‑三(4‑羧基苯氧基)苯;DMF为N,N‑二甲基甲酰胺。该配合物通过溶剂热法制得:将NdCl3·6H2O与H3TCPB配体以1:1的物质的量之比溶于H2O/DMF/乙醇混合溶液中,在水热反应釜中以120℃反应72小时,冷却至室温后收集紫色块状晶体,用蒸馏水洗涤后,真空干燥即可。该配合物结构中包含一维链状双核金属单元,金属Nd3+离子之间表现为反铁磁相互作用;用波长为290nm的光激发该固态配合物,样品可发射较强荧光。因此,该配合物同时具有反铁磁性和荧光性质,是一种潜在的光磁双功能材料。
Description
技术领域
本发明涉及金属配合物,特别涉及一种钕金属配合物,具体属于一种钕离子(III)与1,3,5-三(4-羧基苯氧基)苯和N,N-二甲基甲酰胺构筑的具有光磁性质的配合物及其制备方法和应用。
背景技术
近年来,随着材料科学的不断发展进步,人们已经不再满足于只获得具有单一性质和功能的材料,而是更加青睐于能够获得同时具有两种或两种以上性质和功能的材料,如兼具导电性与磁性、磁-光学性、多孔性与磁性、手性与磁性等,其中集合发光性和磁性的多功能材料是目前很多生产技术的本质所在,具有重要的理论意义和潜在的应用价值。但是由于金属离子和配体之间配位关系的多样化,以及磁相互作用的复杂性,人们对于准确预测配合物结构、光学性质和磁性质之间的关系还存在很大困难,到目前为止,仅有少量这样的材料被报导,所以如何对配体和金属离子进行合理的选择与设计,使其按照期望的方式进行配位,并最终得到目标功能,成为构建此类多功能材料的关键所在。
发明内容
本发明的目的正是针对上述技术现状,提供一种可以作为光磁双功能材料的金属钕配合物及其制备方法和应用。
本发明提供的一种钕配合物,结构简式为:[Nd2(TCPB)2(DMF)(H2O)]n,其中H3TCPB为1,3,5-三(4-羧基苯氧基)苯;DMF为N,N-二甲基甲酰胺。结构式为:
该配合物的晶体属于三斜晶系,P-1空间群,晶胞参数为: α=72.22(3)°,β=85.22(4)°,γ=80.67(4)°。该配合物的不对称结构单元包含一个金属离子Nd3+,一个TCPB3-有机配体,半个配位DMF分子和半个配位水分子。每个Nd3+离子分别与两个TCPB3-配体上的七个氧原子和一个DMF分子(或一个水分子)上的一个氧原子配位,形成八配位十二面体,Nd-O的键长范围为该配合物是一个三维结构。沿a轴方向,相邻的Nd离子通过TCPB3-上的羧基以syn-syn模式进行连接,形成一维金属链结构;随后,一维金属链通过TCPB3-配体相互连接形成三维网络结构。
X射线粉末衍射证实晶体样品均一稳定。通过1000Oe外磁场作用下的变温磁化率实验数据可以得出金属离子间存在反铁磁相互作用,进一步利用居里-韦斯定律对χm -1-T的实验值进行拟合,得到θ=–14.16K,表明配合物中金属离子间存在反铁磁相互作用。室温条件下荧光发射光谱显示,当激发波长为290nm时,配合物的固体可发射较强荧光,荧光强度为配体的两倍。
本发明提供的一种金属钕配合物的制备方法,包括如下步骤:
(1)将摩尔比为1:1的NdCl3·6H2O与H3TCPB,加入到含有体积比为2:3:3的H2O,DMF与乙醇混合溶剂的聚四氟乙烯管中;
(2)将此聚四氟乙烯管置于不锈钢反应釜中密封,在120℃下反应72h,自然冷却至室温,得到紫色块状晶体,用蒸馏水洗涤后真空干燥即可。
本发明的优点和效果:
本发明的金属钕配合物是在溶剂热合成条件下得到,制取工艺简单,产率及纯度较高。
本发明提供的金属钕配合物是基于1,3,5-三(4-羧基苯氧基)苯和N,N-二甲基甲酰胺配体构筑的,该配合物结构中包含一维链状双核金属单元,在1000Oe外磁场下通过变温磁化率实验数据得出金属离子间存在反铁磁相互作用,θ=–14.16K;此外用波长为290nm的光激发该固态配合物,样品可发较强荧光。该配合物同时具有反铁磁性和荧光性质,可用作发光或磁性材料,也可用作光磁双功能材料。
附图说明
图1本发明钕配合物的晶体结构图。图中对称操作代码:A=1-x,1-y,2-z;B=1+x,y,z;C=2-x,2-y,1-z;D=-1+x,y,1+z;E=x,y,1+z;F=-x,1-y,2-z;G=-1+x,-1+y,1+z;H=2-x,1-y,1-z;I=1-x,1-y,1-z。
图2本发明钕配合物在298K的X射线粉末衍射图(实验及模拟图)。
图3本发明钕配合物在1000Oe外磁场作用下的磁性质及其拟合曲线图。
图4本发明钕配合物在298K的固体荧光光谱图
具体实施方式
实施例1.分别称取NdCl3·6H2O(35.3mg,0.1mmol)和H3TCPB(48.6mg,0.1mmol)置于23mL聚四氟乙烯反应釜内衬中,并加入2mL蒸馏水,3mL DMF和3mL无水乙醇,室温条件下搅拌30min后,将其封存在不锈钢反应釜中,在120℃的可控温烘箱中恒温反应72h后,自然冷却至室温,得到满足X-Ray测试要求的紫色块状晶体,用蒸馏水不断净洗并干燥后产率约为42%。
配合物的结构测定:
将晶体样品固定在Bruker SMART 1000 CCD面探衍射仪上,以石墨单色器MoKα为辐射光源,收集样品对波长为的X-Ray衍射数据。以ω扫描方式,衍射数据经LP因子和经验吸收校正。全部X-Ray衍射图还原为衍射指标后,用SHELXTL-NT 5.10版程序包,直接法确定X-Ray衍射强度的位相,初始结构经全矩阵最小二乘法做数轮修正,找出全部非氢原子坐标,确认残余峰不再有非氢原子后,做各向异性温度因子处理。C原子采用理论加氢,水分子中O原子上的氢由差值Fourier合成给出, 并固定在母原子上。详细的晶体测定数据见表1。结构见图1。
表1配合物的晶体学数据
粉末衍射:
X-射线粉末衍射结果表明,晶体样品物相均一,实验衍射图谱与依据晶体结构模拟的粉末衍射图谱一致,见图2。
配合物的磁性质:
变温磁化率与温度的乘积随温度变化的曲线如图3所示,从图中可以看出,在300K时,χmT值为2.97cm3mol-1K,随着温度的降低,χmT值逐渐降低,至2K时降至1.56cm3mol-1K。利用居里-韦斯定律拟合χm -1-T(图3插图),可以得到C=3.05cm3mol-1K,θ=–14.16K,负的θ值表明金属离子间为反铁磁相互作用。
配合物的发光性质:
室温下测定了配体H3TCPB和配合物的固体荧光发射光谱(图4)。从图中可看出,在波长为290nm的光激发下,H3TCPB和配合物在383nm处有较强的发射峰,且配合物的发射峰强度明显强于配体。
Claims (5)
1.一种钕配合物,其特征在于,结构式为:
该配合物的晶体属于三斜晶系,P-1空间群,晶胞参数为: α=72.22(3)°,β=85.22(4)°,γ=80.67(4)°。
2.如权利要求1所述的一种钕配合物的制备方法,其特征在于,包括如下步骤:
(1)将摩尔比为1:1的NdCl3·6H2O与H3TCPB,加入到含有体积比为2:3:3的H2O,DMF与乙醇混合溶剂的聚四氟乙烯管中;
(2)将此聚四氟乙烯管置于不锈钢反应釜中密封,在120℃下反应72小时,自然冷却至室温,得到紫色块状晶体,用蒸馏水洗涤后真空干燥即可。
3.如权利要求1所述的一种钕配合物作为发光材料的应用。
4.如权利要求1所述的一种钕配合物作为磁性材料的应用。
5.如权利要求1所述的一种钕配合物作为光磁双功能材料的应用。
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CN109806912A (zh) * | 2019-03-11 | 2019-05-28 | 山西大学 | 可磁回收的钕配合物/GO/Fe3O4三元复合物及其制备方法和应用 |
CN109806912B (zh) * | 2019-03-11 | 2021-05-14 | 山西大学 | 可磁回收的钕配合物/GO/Fe3O4三元复合物及其制备方法和应用 |
CN112500579A (zh) * | 2020-11-27 | 2021-03-16 | 山西大学 | 一种可磁回收的铈配合物/GO/Fe3O4三元复合物及制备方法和应用 |
CN113372568A (zh) * | 2021-07-05 | 2021-09-10 | 合肥工业大学 | 钕基或钬基手性金属-有机多孔晶态材料的制备方法、制得的材料及其应用 |
CN114716688A (zh) * | 2022-05-17 | 2022-07-08 | 山西大学 | 一种铽配合物及制备方法和应用 |
CN114716688B (zh) * | 2022-05-17 | 2022-12-30 | 山西大学 | 一种铽配合物及制备方法和应用 |
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