具有慢磁弛豫行为的新型单核和双核稀土配合物的研究
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摘要
本论文围绕分子磁性和单分子磁体这一热门研究领域,使用含氮配体和氮氧自由基两类配体,设计合成了26个单、双核稀土配合物。解析了它们的晶体结构,使用元素分析、红外光谱、电子光谱对配合物进行了表征,并对部分配合物进行了光学和磁学性质的测试研究。主要内容包括以下部分：
1.选用四种不同的含氮桥联配体2,2’-联嘧啶(bpm)、1,4-双(2-吡啶基)-2,3-二氮杂-1,3-丁二烯(2-bpdb)、1,4-双(4-吡啶基)-2,3-二氮杂-1,3-丁二烯(4-bpdb)和N-(2-吡啶基甲基)-3-甲氧基-水杨醛亚胺(Hvalampy),设计合成了四个系列双核稀土配合物,磁性测量结果表明其中两例双核稀土Dy2配合物1和3显示出了单分子磁体的磁化强度缓慢弛豫行为,有效能垒分别为37.2K和150.33K。
2.选用单齿含氮配体1,4-双(4-吡啶基)-2,3-二氮杂-1,3-丁二烯(4-bpdb),设计合成了一系列单核稀土配合物。荧光测试和分析观察到单核Eu(Ⅲ)配合物6和Tb(Ⅲ)配合物8的特征荧光跃迁；磁性分析表明单核Dy配合物9有磁化强度缓慢弛豫现象的单分子磁体行为,其有效能垒为23.01K。
3.选用含功能性配位取代基团的间位吡啶基苯基取代的氮氧自由基NIT3Ph3Py为配体得到了一系列的双核四自旋稀土配合物,磁性分析表明该系列配合物中稀土离子和氮氧自由基之间的磁耦合均以铁磁相互作用为主；其中双核Dy2配合物13的交流磁化率显示频率依赖性,表明配合物具有磁化强度缓慢弛豫行为,有效能垒值为3.12K。
4.选用不含功能配位取代基团的对位异丙基苯基取代的氮氧自由基NITPhiPr、正丁基取代的氮氧自由基NITnBu和邻位甲基咪唑基取代的氮氧自由基NITMeIm为配体,合成了三个系列的单核氮氧自由基稀土配合物,并采用近似理论模型对具有旋轨耦合的稀土体系的磁数据进行了初步的分析。
This work focuses on the attractive research fields of molecular magnetism and single-molecule magnets. Choosing the nitrogen-containing ligands and nitronyl nitroxide radicals ligands to coordinate with lanthanide ions, twenty six mononuclear and binuclear lanthanide complexes have been obtained. They have been characterized by X-ray single crystal structure analysis, elemental analyses, IR spectra, electronic spectra, fluorescence spectra and magnetic measurements. Main contents are as following:
1. Four series of binuclear lanthanide complexes have been synthesized by using the different nitrogen-containing ligands of2,2'-bipyrimidine (bpm),1,4-bis(2-pyridyl)-2,3-diaza-1,3-butadiene (2-bpdb),1,4-bis(2-pyridyl)-2,3-diaza-1,3-butadiene (4-bpdb) and N-(2-pyridylmethyl)-3-methoxy-salicylaldiminato (Hvalampy). The magnetic measurements show that the Dy2complex1and3exhibit slow magnetic relaxation and the effective energy barrier of37.2K and150.33K, respectively.
2. A series of mononuclear lanthanide complexes have been synthesized through the reaction of nitrogen-containing ligand (4-bpdb) and lanthanide ions. The Eu(Ⅲ) complex6and Tb(Ⅲ)8exhibit the characteristic fluorescence spectra of the lanthanide ions. The magnetic measurements show that the Dy(Ⅲ) complex9exhibits slow magnetic relaxation and the effective energy barrier of23.01K.
3. A series of four-spin binuclear lanthanide-radical complexes have been synthesized by using3-pyridyl-3-phenyl substituted nitronyl nitroxide radical (NIT3Ph3Py). The magnetic studies show the dominating ferromagnetic interaction between the lanthanide ions and nitroxide radicals within the complexes. The magnetic measurements also show that the Dy(Ⅲ) complex23exhibits slow magnetic relaxation with the effective energy barrier of3.12K.
4. Three series of tri-spin mononuclear lanthanide-radical complexes have been synthesized by using2-isopropyl-phenyl, n-butyl and5-methylimidazole substituted nitronyl nitroxide radicals (NITPhiPr, NITnBu, NITMelm). The approximation model is used to analysis the magnetic data of lanthanide ions with spin-orbit coupling to obtain a reasonable result.
1.选用四种不同的含氮桥联配体2,2’-联嘧啶(bpm)、1,4-双(2-吡啶基)-2,3-二氮杂-1,3-丁二烯(2-bpdb)、1,4-双(4-吡啶基)-2,3-二氮杂-1,3-丁二烯(4-bpdb)和N-(2-吡啶基甲基)-3-甲氧基-水杨醛亚胺(Hvalampy),设计合成了四个系列双核稀土配合物,磁性测量结果表明其中两例双核稀土Dy2配合物1和3显示出了单分子磁体的磁化强度缓慢弛豫行为,有效能垒分别为37.2K和150.33K。
2.选用单齿含氮配体1,4-双(4-吡啶基)-2,3-二氮杂-1,3-丁二烯(4-bpdb),设计合成了一系列单核稀土配合物。荧光测试和分析观察到单核Eu(Ⅲ)配合物6和Tb(Ⅲ)配合物8的特征荧光跃迁；磁性分析表明单核Dy配合物9有磁化强度缓慢弛豫现象的单分子磁体行为,其有效能垒为23.01K。
3.选用含功能性配位取代基团的间位吡啶基苯基取代的氮氧自由基NIT3Ph3Py为配体得到了一系列的双核四自旋稀土配合物,磁性分析表明该系列配合物中稀土离子和氮氧自由基之间的磁耦合均以铁磁相互作用为主；其中双核Dy2配合物13的交流磁化率显示频率依赖性,表明配合物具有磁化强度缓慢弛豫行为,有效能垒值为3.12K。
4.选用不含功能配位取代基团的对位异丙基苯基取代的氮氧自由基NITPhiPr、正丁基取代的氮氧自由基NITnBu和邻位甲基咪唑基取代的氮氧自由基NITMeIm为配体,合成了三个系列的单核氮氧自由基稀土配合物,并采用近似理论模型对具有旋轨耦合的稀土体系的磁数据进行了初步的分析。
This work focuses on the attractive research fields of molecular magnetism and single-molecule magnets. Choosing the nitrogen-containing ligands and nitronyl nitroxide radicals ligands to coordinate with lanthanide ions, twenty six mononuclear and binuclear lanthanide complexes have been obtained. They have been characterized by X-ray single crystal structure analysis, elemental analyses, IR spectra, electronic spectra, fluorescence spectra and magnetic measurements. Main contents are as following:
1. Four series of binuclear lanthanide complexes have been synthesized by using the different nitrogen-containing ligands of2,2'-bipyrimidine (bpm),1,4-bis(2-pyridyl)-2,3-diaza-1,3-butadiene (2-bpdb),1,4-bis(2-pyridyl)-2,3-diaza-1,3-butadiene (4-bpdb) and N-(2-pyridylmethyl)-3-methoxy-salicylaldiminato (Hvalampy). The magnetic measurements show that the Dy2complex1and3exhibit slow magnetic relaxation and the effective energy barrier of37.2K and150.33K, respectively.
2. A series of mononuclear lanthanide complexes have been synthesized through the reaction of nitrogen-containing ligand (4-bpdb) and lanthanide ions. The Eu(Ⅲ) complex6and Tb(Ⅲ)8exhibit the characteristic fluorescence spectra of the lanthanide ions. The magnetic measurements show that the Dy(Ⅲ) complex9exhibits slow magnetic relaxation and the effective energy barrier of23.01K.
3. A series of four-spin binuclear lanthanide-radical complexes have been synthesized by using3-pyridyl-3-phenyl substituted nitronyl nitroxide radical (NIT3Ph3Py). The magnetic studies show the dominating ferromagnetic interaction between the lanthanide ions and nitroxide radicals within the complexes. The magnetic measurements also show that the Dy(Ⅲ) complex23exhibits slow magnetic relaxation with the effective energy barrier of3.12K.
4. Three series of tri-spin mononuclear lanthanide-radical complexes have been synthesized by using2-isopropyl-phenyl, n-butyl and5-methylimidazole substituted nitronyl nitroxide radicals (NITPhiPr, NITnBu, NITMelm). The approximation model is used to analysis the magnetic data of lanthanide ions with spin-orbit coupling to obtain a reasonable result.
引文
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