Fe_3O_4微/纳米磁性材料的合成、自组装及其性能研究
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摘要
微/纳米磁性材料具有独特的结构和优异的性能,有望在电子、信息、自动控制、生物医药等学科领域得到广泛的应用。近几十年来,微/纳米结构磁性材料的制备与性能-直是材料领域的研究热点之一,设计开发具有独特形貌及特殊性能的微/纳米磁性材料是众多研究者的追求目标。
本论文以二茂铁为铁源前驱物、醇/酮为反应介质体系,采用中温溶剂热合成技术,通过调变溶剂体系组成、添加剂种类,优化反应实验参数,成功实现了具有多种形貌特征磁铁矿(Fe3O4)微/纳米晶体及其碳基复合材料的可控制备。利用X-射线衍射(XRD)、57Fe穆斯堡尔谱、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、振动样品磁强计(VSM)等分析技术手段,对微/纳米Fe3O4及其碳基复合材料的物相、组成、形貌、结构进行了系统表征,探讨了不同形貌Fe3O4微米晶的生长机制,研究了合成的Fe3O4及其复合材料的磁性能、以及在电化学电容器和吸附分离领域的基础应用。主要研究结果如下：
1.采用无模板溶剂热技术,以二茂铁为前驱物,成功制得了系列多级分枝结构的星状Fe3O4微米晶体。通过调变反应温度、溶剂种类、前驱物浓度以及反应时间等实验参数,优化了Fe3O4微米晶体生长的反应条件。在350-450℃反应温度范围内,分别选用异丙醇、丙酮、甲醇等为溶剂,利用不同溶剂分子对Fe3O4微晶各界面作用力的差异,调变[100]/[111]晶面的相对生长速率,实现了不同形貌、高度规则对称的六臂二级分枝结构、柱状分枝六角星、金字塔状分枝六足星等Fe3O4微米晶体的可控制备。以上Fe3O4微米晶的形状及磁晶呈现各向异性,与块体磁铁矿相比,具有较高的饱和磁化强度(Ms,90-128emu-g-1)和较大的矫顽力(Hc,223-238Oe)。电化学循环伏安测试表明,Fe3O4六足微米星材料的电化学性能优于通常化学共沉淀法制备的Fe3O4纳米粒子,具有更高的比电容量。
2.利用表面活性剂与不同混合溶剂体系的协同作用,在异丙醇-水及异丙醇-水-表面活性剂溶剂体系中,通过不同构型表面活性剂与Fe304特殊晶面的相互作用强弱差异,调控晶面的相对生长速率,实现了不同形貌、不同尺寸的Fe3O4微/纳米晶体的可控制备,得到了Fe304微纳米八面体(1-2μm)、凹面八面体(2-3μm)、镂空八面体(2-5μm)、微米立方体(1-2μm)等单晶结构,以及由Fe3O4纳米颗粒组装的微米球(1-2μm)多晶磁性材料。研究表明,混合溶剂的组成、水量及表面活性剂的分子结构是影响Fe3O4晶体生长动力学的重要因素。这些微/纳米晶体材料的静磁性能与其尺寸大小和形貌特征密切相关。以上结果表明,在水和表面活性剂参与下,基于异丙醇溶剂的中温溶剂热合成路线可方便实现Fe3O4晶体的形貌控制合成。
3.利用溶剂蒸发诱导组装技术,以晶体硅片为基板、高沸点有机溶剂为介质,通过控制溶剂蒸发过程,实现了Fe3O4六足星状微米晶体的一维线形有序自组装,扫描电镜下首次观察到各向异性的微米级晶体“手拉手”排列；以单晶硅片或涂覆碳膜的铜网为基板、无水乙醇为溶剂,通过缓慢挥发,实现了Fe3Q4微米球的规模化有序组装,可形成一维长程链状(SEM观察)及封闭的环状(TEM观察)自组装结构,为自组装技术应用于磁性微纳米器件的构筑提供了有价值的数据。
4.采用溶剂热合成技术,分别以碳纳米管(CNTs)、氧化石墨烯(GEO)及活性炭(AC)为基体材料,在炭材料表面成功引进磁性纳米粒子,制得Fe304纳米颗粒修饰的碳纳米管(Fe3O4/CNTs)、氧化石墨烯负载高度分散的Fe304纳米颗粒(Fe3O4/GEO)、以及活性炭负载Fe3O4微/纳米球Fe3O4三种复合磁性碳材料。研究了合成过程中溶剂的种类、铁前驱物组成、原料配比、反应温度、反应时间等工艺参数对不同磁性组装体形成的影响,探讨了复合材料的形成机制。磁性能及电化学性能测试表明,随着炭基体性质及其表面负载Fe3O4粒子的尺寸大小、形貌特征与负载量的不同,所制备的三种磁性复合碳材料的饱和磁化强度(Ms)和矫顽力(Hc)显著不同,它们作为超级电容器的正、负极材料表现出不同的氧化、还原规律。此外,磁性活性炭对室温吸附有机污染物罗丹明B显示出较高的吸附脱除效率和良好的再生循环使用性能。
5.以单晶硅为硅源和基板,利用醇-水混合溶剂热体系、二茂铁为铁源,制备得到了含硅的FeSiO3一维纳米材料,长度可达数十微米,平均直径介于20-30nm,具有较窄的尺寸分布。研究了合成反应温度、溶剂组成、反应物浓度等因素对产物形貌的影响,探讨了该一维纳米线的生长机制。FeSiO3一维纳米材料的可控合成为其在固态化学和纳米科学与技术领域的研究及应用创造新机遇。
Owing to the unique structure and excellent properties, micron/nano-magnetic materials are expected to be widely used in electronics, information, automatic control, biomedical and other fields. In the past decades, the preparation of micron/nano-magnetic materials with desired structures and properties has received intensive research interests in the field of materials. More and more researchers are pursuing to design and to develop nano/micron-magnetic materials with controlled structure, unique morphology and outstanding property.
The work in the present thesis mainly focuses on the fabrication of magnetite (Fe3O4) micron/nano-crystals with various novel morphologies via solvothermal synthesis technique. During this process, ferrocene was used as iron source and alcohols/acetone as solvent. By means of manipulating the solvent composition, types of additives, as well as optimization of the experimental parameters, controllable preparation of magnetites and magnetic composites was achieved. The as-prepared products were characterized by using X-ray diffraction, room temperature57Fe Mossbauer spectrum and electron microscopy (SEM, FESEM, TEM), vibrating sample magnetometer (VSM) and FT-IR techniques. Based on the detailed study of the Fe3O4crystals growth process, the possible growth mechanism of Fe3O4micron crystals with different shapes were proposed. Furthermore, the magnetic properties of Fe3O4crystals and their carbon-based composites, the applications in supercapacitor and adsorption/separation have been investigated. The main results are summarized as follows:
(1) We demonstrated that hierarchical branched hexapod magnetite crystals with different morphologies could be prepared through template-free solvothermal route. The reaction condition for Fe3O4hexapod crystal growth is optimized by tuning experimental parameters, including solvent composition, reaction temperature, concentration of ferrocene, as well as reaction duration. In the temperature range of350-450℃, the microstructures of these hexapod Fe3O4micron crystals changed dramatically with the physicochemical properties of the solvents employed such as isopropanol, acetone and methanol. The detailed characterizations reveal that the controllable preparation of highly ordered symmetrical six-arm branched structure, columnar branched hexagonal star, pyramidal branching hexapod Fe3O4micron crystals can be attributed to the changes of fcc Fe3O4nuclei interfacial force derived from different solvent molecules, leading to the modulation of facet [100]/[111] relative growth rate and yielding different morphologies. All these Fe3O4micron crystals, compared to the bulk magnetite, exhibit ferromagnetic behaviors with relatively high saturation magnetization value (Ms,90-128emu·g-1) and coercivity (Hc,223-238Oe) due to their shape anisotropy. The cyclic voltammetry tests show that the electrochemical performance of Fe3O4micron hexapods is superior to that of Fe3O4nanoparticles prepared by general chemical coprecipitation, especially holding a higher specific capacitance.
(2). By taking advantage of the synergistic effect between surfactants and solvent systems, including isopropanol-water and isopropanol-water-surfactant systems, well-defined Fe3O4micron crystals with tailorable size and shape have been successfully fabricated after6h aging at350-400℃by adjusting the experimental conditions. These Fe3O4single crystals are consisted of micrometer scaled octahedrons (1-2μm across), concave octahedrons (2-3μm), octahedral frameworks (2-5μm) and cubes (1-2μm), in addition, polycrystalline microspheres (1-2μm) assembled by Fe3O4nanoparticles were also obtained. From the point of view of crystallography, the diversity of Fe3O4micron crystals should be originated from the varying interaction strength between the surface active agent with different configurations and Fe3O4special facet, the content of water combined with the structure of surfactant is found to play an important role in controlling the kinetic growth process. Moreover, it has also been found that these micrometer sized magnetites exhibit different ferromagnetic properties depending on their sizes and shapes. The results clearly demonstrate that isopropanol-based solvothermal synthesis of magnetite in the presence of water and surfactant is a versatile approach to Fe3O4crystal morphogenesis.
(3). Based on the controllable preparation of magnetite crystals, self-organization of magnetite crystals has been achieved by evaporation-mediated assembly strategy. Quasi one-dimensional "hand-in-hand" self-assembly of the well-defined single crystallined Fe3O4hexapods has been observed for the first time. Besides, the as-made Fe3O4microspheres were assembled into long "necklace" with ethanol as solvent under slow evaporation process. The self-assembled structures of both long-range one-dimensional chain (SEM observation) and a closed ring (TEM observation) can be formed on silicon substrate or TEM copper mesh coated with carbon film. These interesting results could help to lay the foundation for further device applications.
(4). Using one-pot solvothermal synthesis approach, three carbon materials, including carbon nanotubes (CNTs), graphene oxides (GEO) and activated carbon (AC) were decorated with magnetite nanoparticles, and their potential applications in various technological fields were tested. The synthesis parameters, such as the types of solvents and iron precursor, the ratio of raw materials, temperature and reaction time, etc. have been investigated systematically, the formation mechanisms of the composites are also discussed. It has been found that the nature of the carbon matrix and the amount of magnetite nanoparticles deposited on them could affect their magnetic property and electrochemical performance severely, for example the saturation magnetization value (Ms), the coercivity (Hc), as well as the oxidation-reduction function when being used as supercapacitor positive or negative materials. In addition, magnetic activated carbon has been verified to be an excellent adsorbent which exhibits a higher adsorption removal efficiency and good recycling performance for the removal of Rhodamine B in aqueous liquid at room temperature.
(5). Furthermore, iron silicate (FeSiO3) nanowires have been synthesized on silicon substrate via a one-pot solvothermal route without using additional surfactant or template, in which ferrocene serves as iron source and silicon substrate as silicon source, alcohol-water mixture as solvent. The iron silicate nanowires have a width of20-30nm and a length of several ten micrometers. The influences of reaction temperature, solvent composition and concentration of precursor on the morphology of the products have been investigated in detail. A possible growth mechanism of iron silicate nanowires is proposed. We believe that the successful synthesis of iron silicate nanowires with simple method may provide new opportunity for the research and application of this novel1D material in the nanoscience and nanotechnology.
本论文以二茂铁为铁源前驱物、醇/酮为反应介质体系,采用中温溶剂热合成技术,通过调变溶剂体系组成、添加剂种类,优化反应实验参数,成功实现了具有多种形貌特征磁铁矿(Fe3O4)微/纳米晶体及其碳基复合材料的可控制备。利用X-射线衍射(XRD)、57Fe穆斯堡尔谱、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、振动样品磁强计(VSM)等分析技术手段,对微/纳米Fe3O4及其碳基复合材料的物相、组成、形貌、结构进行了系统表征,探讨了不同形貌Fe3O4微米晶的生长机制,研究了合成的Fe3O4及其复合材料的磁性能、以及在电化学电容器和吸附分离领域的基础应用。主要研究结果如下：
1.采用无模板溶剂热技术,以二茂铁为前驱物,成功制得了系列多级分枝结构的星状Fe3O4微米晶体。通过调变反应温度、溶剂种类、前驱物浓度以及反应时间等实验参数,优化了Fe3O4微米晶体生长的反应条件。在350-450℃反应温度范围内,分别选用异丙醇、丙酮、甲醇等为溶剂,利用不同溶剂分子对Fe3O4微晶各界面作用力的差异,调变[100]/[111]晶面的相对生长速率,实现了不同形貌、高度规则对称的六臂二级分枝结构、柱状分枝六角星、金字塔状分枝六足星等Fe3O4微米晶体的可控制备。以上Fe3O4微米晶的形状及磁晶呈现各向异性,与块体磁铁矿相比,具有较高的饱和磁化强度(Ms,90-128emu-g-1)和较大的矫顽力(Hc,223-238Oe)。电化学循环伏安测试表明,Fe3O4六足微米星材料的电化学性能优于通常化学共沉淀法制备的Fe3O4纳米粒子,具有更高的比电容量。
2.利用表面活性剂与不同混合溶剂体系的协同作用,在异丙醇-水及异丙醇-水-表面活性剂溶剂体系中,通过不同构型表面活性剂与Fe304特殊晶面的相互作用强弱差异,调控晶面的相对生长速率,实现了不同形貌、不同尺寸的Fe3O4微/纳米晶体的可控制备,得到了Fe304微纳米八面体(1-2μm)、凹面八面体(2-3μm)、镂空八面体(2-5μm)、微米立方体(1-2μm)等单晶结构,以及由Fe3O4纳米颗粒组装的微米球(1-2μm)多晶磁性材料。研究表明,混合溶剂的组成、水量及表面活性剂的分子结构是影响Fe3O4晶体生长动力学的重要因素。这些微/纳米晶体材料的静磁性能与其尺寸大小和形貌特征密切相关。以上结果表明,在水和表面活性剂参与下,基于异丙醇溶剂的中温溶剂热合成路线可方便实现Fe3O4晶体的形貌控制合成。
3.利用溶剂蒸发诱导组装技术,以晶体硅片为基板、高沸点有机溶剂为介质,通过控制溶剂蒸发过程,实现了Fe3O4六足星状微米晶体的一维线形有序自组装,扫描电镜下首次观察到各向异性的微米级晶体“手拉手”排列；以单晶硅片或涂覆碳膜的铜网为基板、无水乙醇为溶剂,通过缓慢挥发,实现了Fe3Q4微米球的规模化有序组装,可形成一维长程链状(SEM观察)及封闭的环状(TEM观察)自组装结构,为自组装技术应用于磁性微纳米器件的构筑提供了有价值的数据。
4.采用溶剂热合成技术,分别以碳纳米管(CNTs)、氧化石墨烯(GEO)及活性炭(AC)为基体材料,在炭材料表面成功引进磁性纳米粒子,制得Fe304纳米颗粒修饰的碳纳米管(Fe3O4/CNTs)、氧化石墨烯负载高度分散的Fe304纳米颗粒(Fe3O4/GEO)、以及活性炭负载Fe3O4微/纳米球Fe3O4三种复合磁性碳材料。研究了合成过程中溶剂的种类、铁前驱物组成、原料配比、反应温度、反应时间等工艺参数对不同磁性组装体形成的影响,探讨了复合材料的形成机制。磁性能及电化学性能测试表明,随着炭基体性质及其表面负载Fe3O4粒子的尺寸大小、形貌特征与负载量的不同,所制备的三种磁性复合碳材料的饱和磁化强度(Ms)和矫顽力(Hc)显著不同,它们作为超级电容器的正、负极材料表现出不同的氧化、还原规律。此外,磁性活性炭对室温吸附有机污染物罗丹明B显示出较高的吸附脱除效率和良好的再生循环使用性能。
5.以单晶硅为硅源和基板,利用醇-水混合溶剂热体系、二茂铁为铁源,制备得到了含硅的FeSiO3一维纳米材料,长度可达数十微米,平均直径介于20-30nm,具有较窄的尺寸分布。研究了合成反应温度、溶剂组成、反应物浓度等因素对产物形貌的影响,探讨了该一维纳米线的生长机制。FeSiO3一维纳米材料的可控合成为其在固态化学和纳米科学与技术领域的研究及应用创造新机遇。
Owing to the unique structure and excellent properties, micron/nano-magnetic materials are expected to be widely used in electronics, information, automatic control, biomedical and other fields. In the past decades, the preparation of micron/nano-magnetic materials with desired structures and properties has received intensive research interests in the field of materials. More and more researchers are pursuing to design and to develop nano/micron-magnetic materials with controlled structure, unique morphology and outstanding property.
The work in the present thesis mainly focuses on the fabrication of magnetite (Fe3O4) micron/nano-crystals with various novel morphologies via solvothermal synthesis technique. During this process, ferrocene was used as iron source and alcohols/acetone as solvent. By means of manipulating the solvent composition, types of additives, as well as optimization of the experimental parameters, controllable preparation of magnetites and magnetic composites was achieved. The as-prepared products were characterized by using X-ray diffraction, room temperature57Fe Mossbauer spectrum and electron microscopy (SEM, FESEM, TEM), vibrating sample magnetometer (VSM) and FT-IR techniques. Based on the detailed study of the Fe3O4crystals growth process, the possible growth mechanism of Fe3O4micron crystals with different shapes were proposed. Furthermore, the magnetic properties of Fe3O4crystals and their carbon-based composites, the applications in supercapacitor and adsorption/separation have been investigated. The main results are summarized as follows:
(1) We demonstrated that hierarchical branched hexapod magnetite crystals with different morphologies could be prepared through template-free solvothermal route. The reaction condition for Fe3O4hexapod crystal growth is optimized by tuning experimental parameters, including solvent composition, reaction temperature, concentration of ferrocene, as well as reaction duration. In the temperature range of350-450℃, the microstructures of these hexapod Fe3O4micron crystals changed dramatically with the physicochemical properties of the solvents employed such as isopropanol, acetone and methanol. The detailed characterizations reveal that the controllable preparation of highly ordered symmetrical six-arm branched structure, columnar branched hexagonal star, pyramidal branching hexapod Fe3O4micron crystals can be attributed to the changes of fcc Fe3O4nuclei interfacial force derived from different solvent molecules, leading to the modulation of facet [100]/[111] relative growth rate and yielding different morphologies. All these Fe3O4micron crystals, compared to the bulk magnetite, exhibit ferromagnetic behaviors with relatively high saturation magnetization value (Ms,90-128emu·g-1) and coercivity (Hc,223-238Oe) due to their shape anisotropy. The cyclic voltammetry tests show that the electrochemical performance of Fe3O4micron hexapods is superior to that of Fe3O4nanoparticles prepared by general chemical coprecipitation, especially holding a higher specific capacitance.
(2). By taking advantage of the synergistic effect between surfactants and solvent systems, including isopropanol-water and isopropanol-water-surfactant systems, well-defined Fe3O4micron crystals with tailorable size and shape have been successfully fabricated after6h aging at350-400℃by adjusting the experimental conditions. These Fe3O4single crystals are consisted of micrometer scaled octahedrons (1-2μm across), concave octahedrons (2-3μm), octahedral frameworks (2-5μm) and cubes (1-2μm), in addition, polycrystalline microspheres (1-2μm) assembled by Fe3O4nanoparticles were also obtained. From the point of view of crystallography, the diversity of Fe3O4micron crystals should be originated from the varying interaction strength between the surface active agent with different configurations and Fe3O4special facet, the content of water combined with the structure of surfactant is found to play an important role in controlling the kinetic growth process. Moreover, it has also been found that these micrometer sized magnetites exhibit different ferromagnetic properties depending on their sizes and shapes. The results clearly demonstrate that isopropanol-based solvothermal synthesis of magnetite in the presence of water and surfactant is a versatile approach to Fe3O4crystal morphogenesis.
(3). Based on the controllable preparation of magnetite crystals, self-organization of magnetite crystals has been achieved by evaporation-mediated assembly strategy. Quasi one-dimensional "hand-in-hand" self-assembly of the well-defined single crystallined Fe3O4hexapods has been observed for the first time. Besides, the as-made Fe3O4microspheres were assembled into long "necklace" with ethanol as solvent under slow evaporation process. The self-assembled structures of both long-range one-dimensional chain (SEM observation) and a closed ring (TEM observation) can be formed on silicon substrate or TEM copper mesh coated with carbon film. These interesting results could help to lay the foundation for further device applications.
(4). Using one-pot solvothermal synthesis approach, three carbon materials, including carbon nanotubes (CNTs), graphene oxides (GEO) and activated carbon (AC) were decorated with magnetite nanoparticles, and their potential applications in various technological fields were tested. The synthesis parameters, such as the types of solvents and iron precursor, the ratio of raw materials, temperature and reaction time, etc. have been investigated systematically, the formation mechanisms of the composites are also discussed. It has been found that the nature of the carbon matrix and the amount of magnetite nanoparticles deposited on them could affect their magnetic property and electrochemical performance severely, for example the saturation magnetization value (Ms), the coercivity (Hc), as well as the oxidation-reduction function when being used as supercapacitor positive or negative materials. In addition, magnetic activated carbon has been verified to be an excellent adsorbent which exhibits a higher adsorption removal efficiency and good recycling performance for the removal of Rhodamine B in aqueous liquid at room temperature.
(5). Furthermore, iron silicate (FeSiO3) nanowires have been synthesized on silicon substrate via a one-pot solvothermal route without using additional surfactant or template, in which ferrocene serves as iron source and silicon substrate as silicon source, alcohol-water mixture as solvent. The iron silicate nanowires have a width of20-30nm and a length of several ten micrometers. The influences of reaction temperature, solvent composition and concentration of precursor on the morphology of the products have been investigated in detail. A possible growth mechanism of iron silicate nanowires is proposed. We believe that the successful synthesis of iron silicate nanowires with simple method may provide new opportunity for the research and application of this novel1D material in the nanoscience and nanotechnology.
引文
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