3d-4f及4f簇合物的合成与磁性研究
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摘要
单分子磁体是顺磁中心通过有机配体实现磁耦合的一种新型材料。由于结构的特殊性，它们可能呈现出慢磁弛豫、量子隧穿和量子干涉效应等独特的磁现象，使其在量子计算机等方面得到广泛的应用。并且，由于其巨大的比表面积所引起的尺寸效应，以及相应的响应时间、能量损耗、传输效率等方面的改善，使其有望成为实现超高密度信息存储材料。单分子磁体一般是在溶剂或溶剂热等相对温和的条件下以配位化学的方法合成的。因此可以通过分子工程学精心设计合成方法，有目的的控制分子结构，从而改善材料的性能。但是人们对于其特殊磁性产生的机理还不十分清楚，特别是对分子结构与磁性之间关系的研究还很不完善，二者之间还没有完备、系统的定量关系，这大大限制了分子磁体的发展。因此需要合成具有新颖结构的单分子磁体并为其构建理论模型，深入研究已知模型中磁性与结构的关系，这些对实现单分子磁体的定向设计与合成都具有重要意义。本论文共分五章。在第一章的绪论部分，我们介绍了单分子磁体的研究进展、相关物理理论知识以及本课题的选题意义。
第二章中，我们利用相似的配体及金属源通过相同的合成方法得到了三个结构不同但次级结构单元相似的3d-4f簇。其中化合物[Na_2Fe~(III)6Dy~(III)2(N3)_4(HL)4(CH_3O)_4(PhCO_2)6(CH_3OH)2](CH_3OH)3(CH_3CN)2(1)、[Na_2Fe~(III)6Dy~(III)2(N3)_4(L’)4(CH_3O)_4(PhCO_2)6(H2O)2](H2O)2(2)的[Na_2Fe~(III)6Dy~(III)2]核心形成了一对顺反异构体。而且当特戊酸代替苯甲酸时，椅式[Na_2Fe~(III)6Dy~(III)2]簇在化合物[Na_2Fe~(III)6Dy~(III)2(N3)4(L’)4(CH_3O)4(ButCO_2)6](CH_3CN)(3)中通过叠氮相互连接形成了二维菱形网状结构。为了研究3d-4f体系的磁性行为，我们利用Y~(III)离子和Gd~(III)离子代替Dy~(III)离子分别合成了化合物[Na_2Fe~(III)6Y~(III)2(N3)4(L’)_4(CH_3O)_4-(PhCO_2)6(H2O)2](H2O)(4)、[Na_2Fe~(III)6Gd~(III)2(N3)_4(L’)_4(CH_3O)_4(PhCO_2)6(CH_3OH)2]-(H_2O)_6(5)。磁性测试表明，这些化合物都表现出反铁磁性，这主要是因为所有化合物中都含有反铁磁性的[NaFe~(III)_3]单元，而3d-4f和4f-4f之间的相互作用都非常弱。同时除化合物4外，Ln~(III)-Fe~(III)、 Ln~(III)-Ln~(III)之间的相互作用对化合物的磁性有一定的贡献。尽管这些化合物本身不具有单分子磁体性质，但是这些研究发现了一种通过调变配体中的羟基改变顺磁离子簇结构的方法，通过这种方法可能合成新型的3d-4f磁性材料。
第三章中，我们合成了三个氟桥连的镧系金属配合物[Dy~(III)F(oda)(H_2O)3](6)、[Tb~(III)2F2(oda)2(H_2O)2](7)、[Dy~(III)2F2(oda)2(H_2O)2](8)。为了研究桥连F-离子对化合物磁性行为的影响，我们又合成了两个氢氧根桥连的化合物9([Tb~(III)_2(OH)2(oda)2(H_2O)4])、10([Dy~(III)_2(OH)_2(oda)_2(H_2O)4])。直流磁化率测试表明化合物6、7、8中都存在一定的铁磁交换作用，而化合物9、10中只存在反铁磁交换作用；交流磁化率测试表明化合物6、8中存在慢弛豫作用，其他化合物则没有。化合物8、10具有结构相似的Dy2核却表现出完全不同的磁性行为，因此我们推断桥连离子的不同是导致磁性差异的主要原因。与O桥连相比，F-桥连不仅会产生不同的磁相互作用，而且会诱导出慢弛豫作用。这三个氟桥连的镧系金属配合物的成功合成为构筑新的单分子磁体开辟了道路。
第四章中，我们利用8-羟基-2-甲基喹啉(MeQ)为配体通过不同的镧系金属源合成了四个由MeQ桥连的镧系配合物[Gd~(III)2(MeQ)_4(NO_3)_6](11)、[Dy~(III)_2(MeQ)_4(NO_3)_6](12)、[Gd~(III)2(MeQ)_4Cl6](EtOH)_2(13)、[Dy~(III)2(MeQ)_4Cl_6](EtOH)_2(14)。直流磁化率测试显示，这几个化合物都表现出较弱的反铁磁性交换作用。交流磁化率测试表明，化合物12和14都表现出单分子磁体行为，但这两个化合物的弛豫能垒却存在很大差异。这些化合物中的桥连配体是相同的，其键长、键角也相似，因此我们推测在这个体系中，由端基配体改变造成的配位构型及配位场的变化是造成化合物磁性差异的主要原因。虽然端基配体的改变对镧系金属离子间相互作用影响不大，但对其弛豫作用却有很大的影响。这一系列镧系金属配合物的成功合成为研究分子磁体中结构与磁性之间的关系奠定了基础。
Since the dodecanuclear manganese cluster was obtained as the firstsingle-molecule magnet (SMM), SMMs and SCMs (single-chain magnets) have beenof increasing interest, mainly because of their potential applications in high-densitymagnetic memories, quantum computing and molecular spintronics. Over the lasttwo decades, a great number of transition-metal molecular magnets have beensynthesized and their magnetic properties have been widely studied.3In recent years,3d-4f and4f coordination compounds have attracted more and more attention in thefield of molecular magnetism due to their significant magnetic anisotropy from theunquenched orbital angular momentum. In order to investigate the effects of bridgingligands on magnetic behaviors, it is necessary and challenging to explore newsingle-molecule magnets. In the first chapter of five, the concepts, research methods,histories and new developments of single-molecule magnets are introduced. At theend of this chapter, we pointed out the importance of the search project.
In the second charpter, we have shown that the Schiff-base ligands with differentnumbers of hydroxyl can provide access to two unusual polynuclear3d-4f compounds[Na_2Fe~(III)6Dy~(III)2(N_3)4(HL)4(CH_3O)4(PhCO_2)6(CH_3OH)2](CH_3OH)3(CH_3CN)_2(1) and[Na_2Fe~(III)6Dy~(III)2(N_3)4(L’)4(CH_3O)4(PhCO_2)6(H_2O)2](H_2O)2(2), of which the[Na_2Fe~(III)6Dy~(III)2] cores form a couple of cis, trans-isomers. Furthermore, thetrans-[Na_2Fe~(III)6Dy~(III)_2] cluster in compound [Na_2Fe~(III)6Dy~(III)2(N_3)4(L’)4(CH_3O)4-(ButCO_2)6](CH3CN)(3) acts as network nodes in the formation of a2D rhombic grid-like layered structure, when the pivalates take the place of bulkier benzoates. Inorder to investigate the magnetic behaviour of3d-4f systems, compounds[Na2Fe~(III)6Y~(III)2(N3)4(L’)4(CH_3O)4(PhCO2)6(H_2O)_2](H_2O)(4) and [Na2Fe~(III)6Gd~(III)2-(N3)4(L’)4(CH_3O)4(PhCO_2)6(CH_3OH)2](H_2O)6(5) which differ in the lanthanide havealso been prepared. The magnetic properties of these compounds are dominated byantiferromagnetic interactions from [NaFe~(III)3] units, and the interactions between Ln~(III)-Fe~(III)and Ln~(III)-Ln~(III)also make some contributions. To some extent, this researchopens up a promising pathway to investigate the effect of organic ligands on thestructure of polynuclear polymer. Though all the compounds are not SMMsthemselves, the successful synthesis of the compounds may suggest new methods toconstruct novel3d-4f magnetic materials.
In the third chapter, three fluoride-bridged lanthanide compounds[Dy~(III)F(oda)(H_2O)_3](6),[Tb~(III)2F2(oda)2(H_2O)_2](7) and [Dy~(III)2F2(oda)2(H_2O)2](8) havebeen obtained. The magnetic measurements show that the complexes6,7and8exhibit intramolecular ferromagnetic interactions, while only antiferromagneticinteractions are observed in hydroxyl-bridged compounds [Tb~(III)2(OH)2(oda)2(H_2O)4](9) and [Dy~(III)_2(OH)_2(oda)_2(H_2O)_4](10). Among these compounds6and8showfrequency-dependent ac-susceptibility indicative of slow magnetic relaxation.Because the structures of Dy2cores are very similar in compounds8and10, thesesignificant disparities are most likely due to the differences of bridging ligands for therespective dinuclear cores. The bridging F-ions not only promote magnetic exchangeinteractions, but also induce slow magnetic relaxation. We believe that the successfulsynthesis of the three fluoride-bridged coordination compoundes may open up newopportunities to construct SMMs based on fluoride ligand.
In the fourth chapter, three MeQ-bridged lanthanide compounds[Gd~(III)2(MeQ)4(NO_3)6](11),[Dy~(III)2(MeQ)_4(NO_3)_6](12),[Gd~(III)2(MeQ)_4Cl_6](EtOH)_2(13)and [Dy~(III)_2(MeQ)4Cl6](EtOH)_2(14) have been obtained. The magnetic measurementsshow that the complexes exhibit intramolecular antiferromagnetic interactions.Compounds12and14show frequency-dependent ac-susceptibility indicative of slowmagnetic relaxation, but the values of energy barrier are distinct. Because the bridging ligands are very similar in compounds12and14, these significant disparities are mostlikely due to the differences of terminal ligands for the respective dinuclear cores.Although the terminal ligands can not promote magnetic exchange interactionsbetween the lanthanide ions, they can induce slow magnetic relaxation. We believethat the successful synthesis of these compoundes may open up new opportunities toconstruct SMMs.
第二章中，我们利用相似的配体及金属源通过相同的合成方法得到了三个结构不同但次级结构单元相似的3d-4f簇。其中化合物[Na_2Fe~(III)6Dy~(III)2(N3)_4(HL)4(CH_3O)_4(PhCO_2)6(CH_3OH)2](CH_3OH)3(CH_3CN)2(1)、[Na_2Fe~(III)6Dy~(III)2(N3)_4(L’)4(CH_3O)_4(PhCO_2)6(H2O)2](H2O)2(2)的[Na_2Fe~(III)6Dy~(III)2]核心形成了一对顺反异构体。而且当特戊酸代替苯甲酸时，椅式[Na_2Fe~(III)6Dy~(III)2]簇在化合物[Na_2Fe~(III)6Dy~(III)2(N3)4(L’)4(CH_3O)4(ButCO_2)6](CH_3CN)(3)中通过叠氮相互连接形成了二维菱形网状结构。为了研究3d-4f体系的磁性行为，我们利用Y~(III)离子和Gd~(III)离子代替Dy~(III)离子分别合成了化合物[Na_2Fe~(III)6Y~(III)2(N3)4(L’)_4(CH_3O)_4-(PhCO_2)6(H2O)2](H2O)(4)、[Na_2Fe~(III)6Gd~(III)2(N3)_4(L’)_4(CH_3O)_4(PhCO_2)6(CH_3OH)2]-(H_2O)_6(5)。磁性测试表明，这些化合物都表现出反铁磁性，这主要是因为所有化合物中都含有反铁磁性的[NaFe~(III)_3]单元，而3d-4f和4f-4f之间的相互作用都非常弱。同时除化合物4外，Ln~(III)-Fe~(III)、 Ln~(III)-Ln~(III)之间的相互作用对化合物的磁性有一定的贡献。尽管这些化合物本身不具有单分子磁体性质，但是这些研究发现了一种通过调变配体中的羟基改变顺磁离子簇结构的方法，通过这种方法可能合成新型的3d-4f磁性材料。
第三章中，我们合成了三个氟桥连的镧系金属配合物[Dy~(III)F(oda)(H_2O)3](6)、[Tb~(III)2F2(oda)2(H_2O)2](7)、[Dy~(III)2F2(oda)2(H_2O)2](8)。为了研究桥连F-离子对化合物磁性行为的影响，我们又合成了两个氢氧根桥连的化合物9([Tb~(III)_2(OH)2(oda)2(H_2O)4])、10([Dy~(III)_2(OH)_2(oda)_2(H_2O)4])。直流磁化率测试表明化合物6、7、8中都存在一定的铁磁交换作用，而化合物9、10中只存在反铁磁交换作用；交流磁化率测试表明化合物6、8中存在慢弛豫作用，其他化合物则没有。化合物8、10具有结构相似的Dy2核却表现出完全不同的磁性行为，因此我们推断桥连离子的不同是导致磁性差异的主要原因。与O桥连相比，F-桥连不仅会产生不同的磁相互作用，而且会诱导出慢弛豫作用。这三个氟桥连的镧系金属配合物的成功合成为构筑新的单分子磁体开辟了道路。
第四章中，我们利用8-羟基-2-甲基喹啉(MeQ)为配体通过不同的镧系金属源合成了四个由MeQ桥连的镧系配合物[Gd~(III)2(MeQ)_4(NO_3)_6](11)、[Dy~(III)_2(MeQ)_4(NO_3)_6](12)、[Gd~(III)2(MeQ)_4Cl6](EtOH)_2(13)、[Dy~(III)2(MeQ)_4Cl_6](EtOH)_2(14)。直流磁化率测试显示，这几个化合物都表现出较弱的反铁磁性交换作用。交流磁化率测试表明，化合物12和14都表现出单分子磁体行为，但这两个化合物的弛豫能垒却存在很大差异。这些化合物中的桥连配体是相同的，其键长、键角也相似，因此我们推测在这个体系中，由端基配体改变造成的配位构型及配位场的变化是造成化合物磁性差异的主要原因。虽然端基配体的改变对镧系金属离子间相互作用影响不大，但对其弛豫作用却有很大的影响。这一系列镧系金属配合物的成功合成为研究分子磁体中结构与磁性之间的关系奠定了基础。
Since the dodecanuclear manganese cluster was obtained as the firstsingle-molecule magnet (SMM), SMMs and SCMs (single-chain magnets) have beenof increasing interest, mainly because of their potential applications in high-densitymagnetic memories, quantum computing and molecular spintronics. Over the lasttwo decades, a great number of transition-metal molecular magnets have beensynthesized and their magnetic properties have been widely studied.3In recent years,3d-4f and4f coordination compounds have attracted more and more attention in thefield of molecular magnetism due to their significant magnetic anisotropy from theunquenched orbital angular momentum. In order to investigate the effects of bridgingligands on magnetic behaviors, it is necessary and challenging to explore newsingle-molecule magnets. In the first chapter of five, the concepts, research methods,histories and new developments of single-molecule magnets are introduced. At theend of this chapter, we pointed out the importance of the search project.
In the second charpter, we have shown that the Schiff-base ligands with differentnumbers of hydroxyl can provide access to two unusual polynuclear3d-4f compounds[Na_2Fe~(III)6Dy~(III)2(N_3)4(HL)4(CH_3O)4(PhCO_2)6(CH_3OH)2](CH_3OH)3(CH_3CN)_2(1) and[Na_2Fe~(III)6Dy~(III)2(N_3)4(L’)4(CH_3O)4(PhCO_2)6(H_2O)2](H_2O)2(2), of which the[Na_2Fe~(III)6Dy~(III)2] cores form a couple of cis, trans-isomers. Furthermore, thetrans-[Na_2Fe~(III)6Dy~(III)_2] cluster in compound [Na_2Fe~(III)6Dy~(III)2(N_3)4(L’)4(CH_3O)4-(ButCO_2)6](CH3CN)(3) acts as network nodes in the formation of a2D rhombic grid-like layered structure, when the pivalates take the place of bulkier benzoates. Inorder to investigate the magnetic behaviour of3d-4f systems, compounds[Na2Fe~(III)6Y~(III)2(N3)4(L’)4(CH_3O)4(PhCO2)6(H_2O)_2](H_2O)(4) and [Na2Fe~(III)6Gd~(III)2-(N3)4(L’)4(CH_3O)4(PhCO_2)6(CH_3OH)2](H_2O)6(5) which differ in the lanthanide havealso been prepared. The magnetic properties of these compounds are dominated byantiferromagnetic interactions from [NaFe~(III)3] units, and the interactions between Ln~(III)-Fe~(III)and Ln~(III)-Ln~(III)also make some contributions. To some extent, this researchopens up a promising pathway to investigate the effect of organic ligands on thestructure of polynuclear polymer. Though all the compounds are not SMMsthemselves, the successful synthesis of the compounds may suggest new methods toconstruct novel3d-4f magnetic materials.
In the third chapter, three fluoride-bridged lanthanide compounds[Dy~(III)F(oda)(H_2O)_3](6),[Tb~(III)2F2(oda)2(H_2O)_2](7) and [Dy~(III)2F2(oda)2(H_2O)2](8) havebeen obtained. The magnetic measurements show that the complexes6,7and8exhibit intramolecular ferromagnetic interactions, while only antiferromagneticinteractions are observed in hydroxyl-bridged compounds [Tb~(III)2(OH)2(oda)2(H_2O)4](9) and [Dy~(III)_2(OH)_2(oda)_2(H_2O)_4](10). Among these compounds6and8showfrequency-dependent ac-susceptibility indicative of slow magnetic relaxation.Because the structures of Dy2cores are very similar in compounds8and10, thesesignificant disparities are most likely due to the differences of bridging ligands for therespective dinuclear cores. The bridging F-ions not only promote magnetic exchangeinteractions, but also induce slow magnetic relaxation. We believe that the successfulsynthesis of the three fluoride-bridged coordination compoundes may open up newopportunities to construct SMMs based on fluoride ligand.
In the fourth chapter, three MeQ-bridged lanthanide compounds[Gd~(III)2(MeQ)4(NO_3)6](11),[Dy~(III)2(MeQ)_4(NO_3)_6](12),[Gd~(III)2(MeQ)_4Cl_6](EtOH)_2(13)and [Dy~(III)_2(MeQ)4Cl6](EtOH)_2(14) have been obtained. The magnetic measurementsshow that the complexes exhibit intramolecular antiferromagnetic interactions.Compounds12and14show frequency-dependent ac-susceptibility indicative of slowmagnetic relaxation, but the values of energy barrier are distinct. Because the bridging ligands are very similar in compounds12and14, these significant disparities are mostlikely due to the differences of terminal ligands for the respective dinuclear cores.Although the terminal ligands can not promote magnetic exchange interactionsbetween the lanthanide ions, they can induce slow magnetic relaxation. We believethat the successful synthesis of these compoundes may open up new opportunities toconstruct SMMs.
引文
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