氰根桥联多金属配合物分子磁体的磁性研究
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摘要
分子基磁体是以分子或离子为构件的一种磁体材料,其制备采用常规的有机或无机化学合成方法。目前,基于分子水平上的研究、设计和制备主要是针对以有机元素为主的分子磁体材料。与以往的离子型和合金类磁体相比,由于其合成制备条件温和,因此可通过溶液的方法得到。采用含有带磁性的过渡金属或稀土金属离子,和含有有机自由基的基团,并且将两种自旋载体组装而得到的配合物在目前备受关注。同时由于分子合成的无限性和选择的多样性,从而有可能对磁性材料的研究带来大的突破。本文采用穆斯堡尔谱学方法,并结合磁性测量和结构测试等相结合研究了氰根桥联多金属配合物分子磁体的磁性质﹑微观结构和磁耦合相互作用机理等,首次在Ni1.125Co0.375[Fe(CN)6]·6.8H2O中发现自旋玻璃态,并从定性定量角度上对其进行了合理的证实。本论文得到了如下三个方面的研究成果:
1、采用溶液共沉淀法合成了多金属普鲁士蓝类化合物Ni1.125Co0.375[Fe(CN)6]·6.8H2O,获得了从顺磁向铁磁的转变温度大约在16K,拟合得顺磁居里点16.508±0.04K和居里常数3.024±0.03emu.K/mol/Oe。室温下的穆斯堡尔谱测量和红外光谱研究表明金属离子通过氰根成键,即FeⅢ(s=1/2)-CN-(CoⅡ/NiⅡ)(96%)和FeⅢ(s=5/2)-NC-(CoⅡ/NiⅡ)(4%)。
2、直流和交流磁化率的测试中发现Ni1.125Co0.375[Fe(CN)6]·6.8H2O,存在自旋玻璃态,峰位(Tf)移动与频率变化的数量关系,拟合的常数C=0.0081,外推得到零频率下体系的冻结温度为:Tg=13.289K。同时拟合得出特征时间常量τ0=5.62×10-11s,判断因子zv=5.4439。
3、合成一个4f-3d氰根桥联配合物[FeGd(bipy)(H2O)4(CN)6]·5.69H2O,并对样品进行了直流和交流磁性测量,分析结果表明配合物在300K-90K之间是分子内的铁磁性互作用,90K-50K之间可能存在晶体场效应或者自旋交叉行为,50K以下主要以分子间的反铁磁相互作用为主。同时,交流磁化率测量表明配合物不存在磁有序。
最后,我们对本文的工作进行了简要的总结,并对氰根桥联多金属配合物分子磁体这一研究领域的发展前景作了简要的展望。
Molecular-based magnet is one of magnetic material which is composed of molecules or ions, they can be synthesized by conventional organic or inorganic chemical methods. Currently, the research, design and preparation of the molecule-based level mainly lies in the molecule magnetic material and organic elements. Because its synthesis preparation condition is moderate, compared with previous ionic and alloy magnet ,and can be obtained through the solution method. it has attracted considerable attention to complexs which can be assembled by two spin carrier which one contains magnetic of transition metal ion or rare earth metal ions ,and another contains magnetic of organic free radical groups. Additionally, the unlimited of molecular synthesis and the diversity of selection can bring a big breakthrough in the field of magnetic materials. In this thesis, the M?ssbauer measurements, magnetic measurements and structural measurements are performed to study the magnetic properties, microstructure and magnetic coupling mechanism in molecular magnets based on transition metal complexes. We discover the spin-glass-state for the first time in Ni1.125Co0.375[Fe(CN)6]·6.8H2O, which is also confirmed reasonably in terms of the qualitative & quantitive analysis. In the thesis, we have obtained the results in the following three aspects:
1、A multimetallic Prussian blue compound Ni1.125Co0.375[Fe(CN)6]·6.8H2O was prepared by co-precipitation. A transition temperature from ferromagnetic to paramagnetic is about 16K , paramagnetic Curie temperature is 16.508±0.04K, and Curie constant C=3.024±0.03 emu.K/mol/Oe. The room temperature mossbauer spectrum and the infrared spectrum indicated that the metallic ions are bonded through cyanide ligand, i.e.: FeⅢ(s=1/2)-CN-(CoⅡ/NiⅡ)(96%) and FeⅢ(s=5/2)-NC-(CoⅡ/NiⅡ) (4%).
2、The measurement of direct-current and alternating-current magnetic susceptibility indicated that the spin-glass-state exists in the Ni1.125Co0.375[Fe(CN)6]·6.8H2O. The dependence of peak position (Tf) on the frequency shift is also found with the fitting constant C=0.0081, by extrapolation under the zero frequency system's freezing temperatures is Tg=13.289K. Simultaneously we have gotten the characteristic time constantτ0=5.62×10-11s and judgment factor zv=5.4439.
3、A 4f-3d cyanide ligand complex [FeGd(bipy)(H2O)4(CN)6]·5.69H2O was synthesized, which is executed on direct-current and alternating-current magnetization process. The analysis belongs to intramolecular ferromagnetic interaction in 300K-90K, about crystalline field effects or spin-crossover in 90K-50K and intermolecular antiferromagnetic interaction below 50K. At the same time, the alternating-current magnetic susceptibility indicated that magnetic ordering didn’t exist the complex.
At last, we summarize the work in the thesis and discuss the prospects of the study of molecular magnets based on multi metal complexes by cyanides.
1、采用溶液共沉淀法合成了多金属普鲁士蓝类化合物Ni1.125Co0.375[Fe(CN)6]·6.8H2O,获得了从顺磁向铁磁的转变温度大约在16K,拟合得顺磁居里点16.508±0.04K和居里常数3.024±0.03emu.K/mol/Oe。室温下的穆斯堡尔谱测量和红外光谱研究表明金属离子通过氰根成键,即FeⅢ(s=1/2)-CN-(CoⅡ/NiⅡ)(96%)和FeⅢ(s=5/2)-NC-(CoⅡ/NiⅡ)(4%)。
2、直流和交流磁化率的测试中发现Ni1.125Co0.375[Fe(CN)6]·6.8H2O,存在自旋玻璃态,峰位(Tf)移动与频率变化的数量关系,拟合的常数C=0.0081,外推得到零频率下体系的冻结温度为:Tg=13.289K。同时拟合得出特征时间常量τ0=5.62×10-11s,判断因子zv=5.4439。
3、合成一个4f-3d氰根桥联配合物[FeGd(bipy)(H2O)4(CN)6]·5.69H2O,并对样品进行了直流和交流磁性测量,分析结果表明配合物在300K-90K之间是分子内的铁磁性互作用,90K-50K之间可能存在晶体场效应或者自旋交叉行为,50K以下主要以分子间的反铁磁相互作用为主。同时,交流磁化率测量表明配合物不存在磁有序。
最后,我们对本文的工作进行了简要的总结,并对氰根桥联多金属配合物分子磁体这一研究领域的发展前景作了简要的展望。
Molecular-based magnet is one of magnetic material which is composed of molecules or ions, they can be synthesized by conventional organic or inorganic chemical methods. Currently, the research, design and preparation of the molecule-based level mainly lies in the molecule magnetic material and organic elements. Because its synthesis preparation condition is moderate, compared with previous ionic and alloy magnet ,and can be obtained through the solution method. it has attracted considerable attention to complexs which can be assembled by two spin carrier which one contains magnetic of transition metal ion or rare earth metal ions ,and another contains magnetic of organic free radical groups. Additionally, the unlimited of molecular synthesis and the diversity of selection can bring a big breakthrough in the field of magnetic materials. In this thesis, the M?ssbauer measurements, magnetic measurements and structural measurements are performed to study the magnetic properties, microstructure and magnetic coupling mechanism in molecular magnets based on transition metal complexes. We discover the spin-glass-state for the first time in Ni1.125Co0.375[Fe(CN)6]·6.8H2O, which is also confirmed reasonably in terms of the qualitative & quantitive analysis. In the thesis, we have obtained the results in the following three aspects:
1、A multimetallic Prussian blue compound Ni1.125Co0.375[Fe(CN)6]·6.8H2O was prepared by co-precipitation. A transition temperature from ferromagnetic to paramagnetic is about 16K , paramagnetic Curie temperature is 16.508±0.04K, and Curie constant C=3.024±0.03 emu.K/mol/Oe. The room temperature mossbauer spectrum and the infrared spectrum indicated that the metallic ions are bonded through cyanide ligand, i.e.: FeⅢ(s=1/2)-CN-(CoⅡ/NiⅡ)(96%) and FeⅢ(s=5/2)-NC-(CoⅡ/NiⅡ) (4%).
2、The measurement of direct-current and alternating-current magnetic susceptibility indicated that the spin-glass-state exists in the Ni1.125Co0.375[Fe(CN)6]·6.8H2O. The dependence of peak position (Tf) on the frequency shift is also found with the fitting constant C=0.0081, by extrapolation under the zero frequency system's freezing temperatures is Tg=13.289K. Simultaneously we have gotten the characteristic time constantτ0=5.62×10-11s and judgment factor zv=5.4439.
3、A 4f-3d cyanide ligand complex [FeGd(bipy)(H2O)4(CN)6]·5.69H2O was synthesized, which is executed on direct-current and alternating-current magnetization process. The analysis belongs to intramolecular ferromagnetic interaction in 300K-90K, about crystalline field effects or spin-crossover in 90K-50K and intermolecular antiferromagnetic interaction below 50K. At the same time, the alternating-current magnetic susceptibility indicated that magnetic ordering didn’t exist the complex.
At last, we summarize the work in the thesis and discuss the prospects of the study of molecular magnets based on multi metal complexes by cyanides.
引文
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