无机层状纳米材料的制备表征与应用（BN，MoS_2）
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摘要
无机层状纳米材料具有广阔的应用前景,是一类具有特殊结构和性能的新型纳米功能材料,也是目前化学与材料研究领域的前沿与热点。本论文旨在探索采用简便的化学原理和制备方法合成具有空心特征的层状无机纳米材料并探究所制备的无机空心层状微纳米材料的形成机制与潜在应用,取得了一系列的创新性成果。本论文提出了在固相高温高压体系中制备亚微米级氮化硼空心格子的反应机制,对所合成的六方相氮化硼空心格子进行催化剂的负载并对该复合体系的光催化性能进行了初步探讨。本论文还研究了由液相溶剂热合成的纳米片自组装的二硫化钼(MoS2)层级空心结构,包括层级结构的MoS2空心球和MoS2空心管,探索了它们的形成机制和结构特点。同时主要研究了所制备的MoS2空心球和空心管在锂离子电池负极材料方面的应用。论文主要内容归纳如下：
1在本章研究中,六方相的氮化硼亚微米级空心格子(BNMB)通过选择KBH4, NH4F和Zn粉做为反应物在450℃反应20h制得.原产物的形成过程通过XRD,TEM和EDS分析得出反应过程中原位生成的立方相的KZnF3中间体作为模板形成BNMB。由于所制备的BNMB具有独特的结构特征,高的比表面积以及优异的化学稳定性被用作催化剂载体。在接下来的实验中采用一种简单的湿化学法制备出SnO2/BNMB复合材料。这种复合材料的紫外漫反射光谱显示其吸收边缘在～470nm,使其有望在光催化反应中得到应用。实验结果表明SnO2/BNMB在催化降解甲基橙(MO)时显示了优异的光催化活性,在可见光的照射下,30min降解率达到92%。这种良好的光催化活性主要是由于材料较窄的带隙,对MO强的吸附能力以及在SnO2/BNMB界面对电荷的有效分离。
2由于MoS2具有的层状结构和高的理论比容量,被认为是一种潜在的锂离子电池负极材料。但是由于低的电导率,使其循环稳定性和倍率性能较差。在本章工作中,通过一种简单有效的合成方法得到分子层间距增加的纳米片自组装的层级MoS2空心球,这些空心球的尺寸在400～800nm左右。MoS2的层级空心结构的形成机制基于一种中间产物K2NaMoO3F3作为自牺牲模板成功制备。所获得的层级MoS2空心球状颗粒在锂离子电池性能测试中显示了优异的电化学性能,在100mAg-1的电流密度下80个循环后容量仍能维持在902mAh g-1,当电流密度1000mAg-1时,容量为780mAh g-1,具备较好的倍率性能。所制备的MoS2电极材料的锂离子脱嵌行为被研究。此外基于实验结果,所制备的层级MoS2空心球作为电极材料良好性能的原因也进行了初步的探讨主要归因于材料的层级结构和空心特征,S-Mo-S分子层增加的层间距以及较高的比表面积。
3目前为止,MoS2空心管的研究还比较少,相关的报道往往存在制备工艺苛刻、较高的成本以及对环境污染比较严重等问题。本章工作通过一种温和的溶剂热方法制备出大量的由纳米片自组装的MoS2层级管状空心结构。在制备过程中通过加入MnCl2·4H2O形成棒状结构的MnMoO4。在反应过程中,棒状结构的MnMoO4不仅提供钼源同时还作为形成管状空心结构的自牺牲模板。这种褶皱状的表面结合其空心特征不仅有利于材料与电解液的接触使Li+有效的脱嵌,还可以在充放电过程中使其体积膨胀得到一定的缓冲进而增强其循环性能。其电化学性能测试显示了较高的储锂能力和较好的循环稳定性。这种层级管状结构的1D纳米材料是纳米片和纳米管的结合,具有较大的比表面积允许电解液中的Li+与活性物质充分有效接触、缩短了电荷的传输距离、并且1D的纳米结构用作电极材料被认为是有利于电子的传输,因此显示了较好的倍率性能。
Inorganic layer hollow materials have many promising applications based on their unique structure and special properties. They are the front and hot research fields of chemistry and materials currently. The goal of this dissertation is to explore the facile chemistry principle and synthesis approach to obtain inorganic hollow nano/micro materials and further study their application. The innovative achievements of this dissertation include:propose the reaction mechanism of synthesis of novel boron nitride submicro-boxes in solid-phase system under high-temperature and high-pressure environments. SnO2photocatalyst was deposited on BNMB by a simple wet chemistry method and the photocatalytic performance of SnO2/BNMB has been investigated. This dissertation also prepare the MoS2hierarchical hollow structures, hollow spheres and tubes, which assembled by nanosheets synthesized by the liquid-phase solvothermal technique. We explore the possible formation mechanisms, structural features and their lithium storage performance of the MoS2hierarchical hollow structures. Thesis is summarized as follows:
1In this study, hexagonal boron nitride submicro-boxes (BNMB)(0.50～1.4μm) have been synthesized by using KBH4, NH4F and Zn in a stainless steel autoclave at450℃. The formation process was studied by XRD, TEM and EDS, and it is considered that the in situ formed KZnF3intermediate cubes serve as templates for the formation of BNMB. The as-formed BNMB, with unique structural features, high specific surface area and good chemical properties, can be applied as a catalyst support for SnO2. The UV-Vis diffuse reflectance spectrum of SnO2/BNMB shows the absorption edge in the visible region (-470run), making it suitable for photocatalytic application. The experimental result indicates that the SnO2/BNMB exhibited excellent photocatalytic activity on the degradation of methyl orange (MO), which was up to92%after30min of visible-light irradiation. The good photocatalytic activity was attributed mainly to its suitable band gap energy, strong adsorption ability for MO, and effective charge separation at the SnO2/BNMB photocatalyst interface.
2MoS2, due to its layered structure and high theoretical capacity, has been regarded as a potential candidate for electrode materials in lithium secondary batteries. But it suffers from the poor cycling stability and low rate capability. Here, hierarchical hollow nanoparticles of MoS2, with the diameter of400～800μm, assembled by increased interlayer-distance nanosheets are synthesized by a simple solvothermal reaction at a low temperature. The formation of hierarchical hollow nanoparticles is based on the intermediate, K2NaMoO3F3, as a self-sacrificed template. These hollow nanoparticles exhibit a reversible capacity of902mAh g-1at100mA g-1after80cycles, much higher than the solid counterparts. At a current density of1000mA g-1, the reversible capacity of the hierarchical hollow nanoparticles could be still maintained at780mAh g-1. The enhanced lithium storage performances of the hierarchical hollow nanoparticles in reversible capacities, cycling stability and rate performances can be attributed to their hierarchical surface, hollow structure feature and increased layer distance of S-Mo-S. Hierarchical hollow nanoparticles as an ensemble of these features, could be applied to other electrode materials for the superior electrochemical performance.
3Hierarchical hollow nanotubes assembled by nanosheets have been fabricated in high yield by a mild solvothermal route at low temperature. A possible formation mechanism of the samples was also proposed. During the reaction process, the MnMo04nanorods were firstly formed at a lower temperature, in which the intermediate crystals resulted from the reaction between MoO42-and Mn2+and formed in-situ and then served as the self-sacrificed template. The highly wrinkled surface combined with the hollow structure would offer a huge specific surface area for electrochemical reactions, which benefits the electrode material to interact effectively with the Li+in the electrolyte and shorten the diffusion length of the charge carriers. Meanwhile, there are much empty space in this electrode material, which can effectively tolerate the volume change during the discharge/charge processes. Furthermore, the introduction of hollow channel inside the1D nanostructures can enhance the effective interaction and reduce the diffusion distance of lithium ions between the electrolyte and the electrode. The hierarchical hollow nanotubes show the better electrochemical performance.
1在本章研究中,六方相的氮化硼亚微米级空心格子(BNMB)通过选择KBH4, NH4F和Zn粉做为反应物在450℃反应20h制得.原产物的形成过程通过XRD,TEM和EDS分析得出反应过程中原位生成的立方相的KZnF3中间体作为模板形成BNMB。由于所制备的BNMB具有独特的结构特征,高的比表面积以及优异的化学稳定性被用作催化剂载体。在接下来的实验中采用一种简单的湿化学法制备出SnO2/BNMB复合材料。这种复合材料的紫外漫反射光谱显示其吸收边缘在～470nm,使其有望在光催化反应中得到应用。实验结果表明SnO2/BNMB在催化降解甲基橙(MO)时显示了优异的光催化活性,在可见光的照射下,30min降解率达到92%。这种良好的光催化活性主要是由于材料较窄的带隙,对MO强的吸附能力以及在SnO2/BNMB界面对电荷的有效分离。
2由于MoS2具有的层状结构和高的理论比容量,被认为是一种潜在的锂离子电池负极材料。但是由于低的电导率,使其循环稳定性和倍率性能较差。在本章工作中,通过一种简单有效的合成方法得到分子层间距增加的纳米片自组装的层级MoS2空心球,这些空心球的尺寸在400～800nm左右。MoS2的层级空心结构的形成机制基于一种中间产物K2NaMoO3F3作为自牺牲模板成功制备。所获得的层级MoS2空心球状颗粒在锂离子电池性能测试中显示了优异的电化学性能,在100mAg-1的电流密度下80个循环后容量仍能维持在902mAh g-1,当电流密度1000mAg-1时,容量为780mAh g-1,具备较好的倍率性能。所制备的MoS2电极材料的锂离子脱嵌行为被研究。此外基于实验结果,所制备的层级MoS2空心球作为电极材料良好性能的原因也进行了初步的探讨主要归因于材料的层级结构和空心特征,S-Mo-S分子层增加的层间距以及较高的比表面积。
3目前为止,MoS2空心管的研究还比较少,相关的报道往往存在制备工艺苛刻、较高的成本以及对环境污染比较严重等问题。本章工作通过一种温和的溶剂热方法制备出大量的由纳米片自组装的MoS2层级管状空心结构。在制备过程中通过加入MnCl2·4H2O形成棒状结构的MnMoO4。在反应过程中,棒状结构的MnMoO4不仅提供钼源同时还作为形成管状空心结构的自牺牲模板。这种褶皱状的表面结合其空心特征不仅有利于材料与电解液的接触使Li+有效的脱嵌,还可以在充放电过程中使其体积膨胀得到一定的缓冲进而增强其循环性能。其电化学性能测试显示了较高的储锂能力和较好的循环稳定性。这种层级管状结构的1D纳米材料是纳米片和纳米管的结合,具有较大的比表面积允许电解液中的Li+与活性物质充分有效接触、缩短了电荷的传输距离、并且1D的纳米结构用作电极材料被认为是有利于电子的传输,因此显示了较好的倍率性能。
Inorganic layer hollow materials have many promising applications based on their unique structure and special properties. They are the front and hot research fields of chemistry and materials currently. The goal of this dissertation is to explore the facile chemistry principle and synthesis approach to obtain inorganic hollow nano/micro materials and further study their application. The innovative achievements of this dissertation include:propose the reaction mechanism of synthesis of novel boron nitride submicro-boxes in solid-phase system under high-temperature and high-pressure environments. SnO2photocatalyst was deposited on BNMB by a simple wet chemistry method and the photocatalytic performance of SnO2/BNMB has been investigated. This dissertation also prepare the MoS2hierarchical hollow structures, hollow spheres and tubes, which assembled by nanosheets synthesized by the liquid-phase solvothermal technique. We explore the possible formation mechanisms, structural features and their lithium storage performance of the MoS2hierarchical hollow structures. Thesis is summarized as follows:
1In this study, hexagonal boron nitride submicro-boxes (BNMB)(0.50～1.4μm) have been synthesized by using KBH4, NH4F and Zn in a stainless steel autoclave at450℃. The formation process was studied by XRD, TEM and EDS, and it is considered that the in situ formed KZnF3intermediate cubes serve as templates for the formation of BNMB. The as-formed BNMB, with unique structural features, high specific surface area and good chemical properties, can be applied as a catalyst support for SnO2. The UV-Vis diffuse reflectance spectrum of SnO2/BNMB shows the absorption edge in the visible region (-470run), making it suitable for photocatalytic application. The experimental result indicates that the SnO2/BNMB exhibited excellent photocatalytic activity on the degradation of methyl orange (MO), which was up to92%after30min of visible-light irradiation. The good photocatalytic activity was attributed mainly to its suitable band gap energy, strong adsorption ability for MO, and effective charge separation at the SnO2/BNMB photocatalyst interface.
2MoS2, due to its layered structure and high theoretical capacity, has been regarded as a potential candidate for electrode materials in lithium secondary batteries. But it suffers from the poor cycling stability and low rate capability. Here, hierarchical hollow nanoparticles of MoS2, with the diameter of400～800μm, assembled by increased interlayer-distance nanosheets are synthesized by a simple solvothermal reaction at a low temperature. The formation of hierarchical hollow nanoparticles is based on the intermediate, K2NaMoO3F3, as a self-sacrificed template. These hollow nanoparticles exhibit a reversible capacity of902mAh g-1at100mA g-1after80cycles, much higher than the solid counterparts. At a current density of1000mA g-1, the reversible capacity of the hierarchical hollow nanoparticles could be still maintained at780mAh g-1. The enhanced lithium storage performances of the hierarchical hollow nanoparticles in reversible capacities, cycling stability and rate performances can be attributed to their hierarchical surface, hollow structure feature and increased layer distance of S-Mo-S. Hierarchical hollow nanoparticles as an ensemble of these features, could be applied to other electrode materials for the superior electrochemical performance.
3Hierarchical hollow nanotubes assembled by nanosheets have been fabricated in high yield by a mild solvothermal route at low temperature. A possible formation mechanism of the samples was also proposed. During the reaction process, the MnMo04nanorods were firstly formed at a lower temperature, in which the intermediate crystals resulted from the reaction between MoO42-and Mn2+and formed in-situ and then served as the self-sacrificed template. The highly wrinkled surface combined with the hollow structure would offer a huge specific surface area for electrochemical reactions, which benefits the electrode material to interact effectively with the Li+in the electrolyte and shorten the diffusion length of the charge carriers. Meanwhile, there are much empty space in this electrode material, which can effectively tolerate the volume change during the discharge/charge processes. Furthermore, the introduction of hollow channel inside the1D nanostructures can enhance the effective interaction and reduce the diffusion distance of lithium ions between the electrolyte and the electrode. The hierarchical hollow nanotubes show the better electrochemical performance.
引文
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