功能配合物的探索合成与磁场对结构的影响研究
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摘要
分子基材料,特别是配合物型分子基材料,由于其结构多样和在催化、光、电、磁等方面都具有潜在的应用前景,在近年来材料科学的研究中已成为非常受重视的新兴科学领域。目前分子基磁体大都是通过自组装反应合成得到的,自组装反应大多取决于内驱动力,人为很难控制。而磁场作为一种外动力,已经证明能够被用来作为自组装的动力,用来控制排列和自组装的反应,得到有序材料,甚至能对产物进行选择性的合成。所以,我们认为在分子磁体的自组装过程中引入外加磁场则有可能对这些有顺磁性离子参与的超分子自组装反应产生一定的影响,甚至控制这些自组装反应方向,增强分子磁体的磁交换作用和改善磁性能等。此外,配合物型分子基材料具有结构多样性的特点,易于用化学方法在分子水平上对其进行修饰和剪裁而提高或改变其磁性能,这种分子水平上的剪裁和修饰也可以得到多功能性的分子材料。论文详细内容归纳如下:
1.成功地观测到磁场对分子磁体的结晶行为的影响。实验结果清楚地显示,磁场下合成的分子磁体分子间的磁相互作用明显增强,自旋倾斜角度显著减小,进而引起磁有序温度、剩余磁矩、矫顽场等各项性质的改变。这些结果说明外加磁场能有效影响自旋离子的取向,促进自旋有序状态的生成。
2.叠氮离子N~(3-)因其丰富的桥联模式和有效的磁传递性在配合物的构筑中得到广泛应用。利用salophen有机辅助配体合成了一个多核叠氮化合物。单晶结构解析表明,三核簇内包含EO叠氮桥联和叠氮端基配位两种配位方式,三核簇之间通过氢键和π-π作用构成超分子网络。
3.选取四氮唑作为配体,通过控制水热条件,合成出微孔三维配位聚合物晶体。结构测试表明其具有穿插的金刚石结构。还进行了详细的性质表征,包括元素分析,红外,热分析等。
Great efforts have been expended on crystal engineering of molecular based materials,especially coordination polymers,because of their fascinating structural diversity and potential applications in catalysis,luminescense,magnetism and porosity.Self-assembly method is the main synthetic strategy of molecule-based magnetic materials.The self-assembly reaction mainly depends on inner driving forces,which is difficult to control.However,as kind of exterior driving forces, magnetic field has been proved that it can be used as driving force in self-assembly reactions.Some products can be orientated and assembled to form ordered structure induced by external magnetic field.Also,the magnetic field can change the final products in some chemical reactions.Based on the above facts,it is believed that the supramolecular self-assembly involved paramagnetic metal ions reaction toward molecule-based magnet can be influenced by external magnetic field.It is also presumed that applied magnetic field can control the final products or enhance the magnetism of magnetic products.In addition,molecule-based materials with diversity of structural features can be modified and redesigned in molecular structure, which will be helpful to obtain multifunctional molecular materials.The main parts of the dissertation are summarized below:
1.The magnetic field effect on the crystallization of molecule-based magnet is observed.It is clearly shown that the molecular magnet with an improved antiferrimagnetic coupling interaction and a smaller spin canting angle can be obtained under a 0.20 T applied magnetic field,which cause the change in ordering temperature,remnant moment and coercive field.The results indicate that magnetic field can influence the orientation of magnetic ions and accelerate the more ordered state of spins.
2.The azido ion as a bridge has been an intriguing synthetic approach to molecular- based magnetic materials,due to their remarkable diversities in structural and magnetic behaviors.One polymeric Co~Ⅲ-azido coordination polymer with the tetradentate Schiff base salophen as co-ligand has been synthesized and characterized by single crystal X-ray diffraction.Two azide ligand acts with the end-on bridging coordination mode between Co(Ⅲ) and Na(Ⅰ) ions and one as a terminal ligand.The Compound has a supramolecular structure with hydrogen bond andπ-πinteraction.
3.A 3D framework structure based on tetrazole and transition metals has been synthesized under hydrothermal conditions,which has the interpenetrating diamond-like supramolecular topology and is further characterized by FI-IR, elemental analysis and thermogravimetric analysis.
1.成功地观测到磁场对分子磁体的结晶行为的影响。实验结果清楚地显示,磁场下合成的分子磁体分子间的磁相互作用明显增强,自旋倾斜角度显著减小,进而引起磁有序温度、剩余磁矩、矫顽场等各项性质的改变。这些结果说明外加磁场能有效影响自旋离子的取向,促进自旋有序状态的生成。
2.叠氮离子N~(3-)因其丰富的桥联模式和有效的磁传递性在配合物的构筑中得到广泛应用。利用salophen有机辅助配体合成了一个多核叠氮化合物。单晶结构解析表明,三核簇内包含EO叠氮桥联和叠氮端基配位两种配位方式,三核簇之间通过氢键和π-π作用构成超分子网络。
3.选取四氮唑作为配体,通过控制水热条件,合成出微孔三维配位聚合物晶体。结构测试表明其具有穿插的金刚石结构。还进行了详细的性质表征,包括元素分析,红外,热分析等。
Great efforts have been expended on crystal engineering of molecular based materials,especially coordination polymers,because of their fascinating structural diversity and potential applications in catalysis,luminescense,magnetism and porosity.Self-assembly method is the main synthetic strategy of molecule-based magnetic materials.The self-assembly reaction mainly depends on inner driving forces,which is difficult to control.However,as kind of exterior driving forces, magnetic field has been proved that it can be used as driving force in self-assembly reactions.Some products can be orientated and assembled to form ordered structure induced by external magnetic field.Also,the magnetic field can change the final products in some chemical reactions.Based on the above facts,it is believed that the supramolecular self-assembly involved paramagnetic metal ions reaction toward molecule-based magnet can be influenced by external magnetic field.It is also presumed that applied magnetic field can control the final products or enhance the magnetism of magnetic products.In addition,molecule-based materials with diversity of structural features can be modified and redesigned in molecular structure, which will be helpful to obtain multifunctional molecular materials.The main parts of the dissertation are summarized below:
1.The magnetic field effect on the crystallization of molecule-based magnet is observed.It is clearly shown that the molecular magnet with an improved antiferrimagnetic coupling interaction and a smaller spin canting angle can be obtained under a 0.20 T applied magnetic field,which cause the change in ordering temperature,remnant moment and coercive field.The results indicate that magnetic field can influence the orientation of magnetic ions and accelerate the more ordered state of spins.
2.The azido ion as a bridge has been an intriguing synthetic approach to molecular- based magnetic materials,due to their remarkable diversities in structural and magnetic behaviors.One polymeric Co~Ⅲ-azido coordination polymer with the tetradentate Schiff base salophen as co-ligand has been synthesized and characterized by single crystal X-ray diffraction.Two azide ligand acts with the end-on bridging coordination mode between Co(Ⅲ) and Na(Ⅰ) ions and one as a terminal ligand.The Compound has a supramolecular structure with hydrogen bond andπ-πinteraction.
3.A 3D framework structure based on tetrazole and transition metals has been synthesized under hydrothermal conditions,which has the interpenetrating diamond-like supramolecular topology and is further characterized by FI-IR, elemental analysis and thermogravimetric analysis.
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