氯化氧铋及锰基化合物微纳米结构的液相合成及储能性质研究
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摘要
本论文旨在探索储能材料BiOCl以及Mn基化合物的控制合成及性能研究。溶剂热条件下控制合成了均一的3D BiOCl微结构,结合其层状结构的特点,研究了电化学储氢性能；并通过溶剂热-前驱物后处理的方式合成了多孔的Mn02片状和球状结构,以及多孔的MnCo2O4和CoMn2O4空心球结构,在纽扣电池模型中研究了其作为锂电池负极材料的电化学性质。本论文的主要内容可以归纳如下：
1、采用溶剂热法选择性合成了3D的BiOCl微米结构,如2.5μm的牡丹花状,1μm的球花状和3μm的粗糙球状结构。这些结构分别由直径1000nm,300nm,200nm的片堆积而成,表征发现片的生长面均是(001)。基于不同反应时间的产品表征结果,我们提出了“快速成核-定向排列-边界融合”的生长过程。N2吸附脱附曲线表明粗糙球结构具有最大的比表面积数据和孔体积数据,这影响其电化学储氢的性能。电化学储氢测试表明有较大比表面和孔体积的样品具有更大的储氢容量值。考虑到其(001)面较大的层间距,我们推测(001)面的层间空隙储存活性H。此外,我们还研究了生长面为[2(-)21]法向的纳米片堆积而成的微米球结构,结果进一步证实了活性H进入了BiOCl的层间。相关实验结果发表在杂志Journal of Nanoscience and Nanotechnology上。
2、分别在表面活性剂十二烷基苯磺酸钠(SDBS)和十二烷基磺酸钠(SDS)的辅助下,直径2.3μm厚度200nm的均匀微米片和由厚度50nm的纳米片堆积而成的直径3.1μm的花状球结构的MnCO3,在水热条件下合成出来。合成的MnCO3经400℃煅烧4小时,我们得到了多孔的的y-MnO2片状和花球状结构。前者具有更窄的孔径分布以及更大的比表面积,更利于Li+的存储和传输,而表现出了优良的储锂性能。测试结果显示在100mA/g的电流密度下两种结构的首次放电容量分别为1997mAh/g和1533mAh/g。值得指出的是,γ-MnO2多孔片状结构经100次循环后,其容量仍然保持在626mAh/g,呈现了较优良的循环性能。该项研究成果发表在Journal of Alloys and Compounds上。
3、通过控制反应物Mn/Co的摩尔比,利用热解碳酸盐前驱体的方法,选择性合成了MnCO2O4和CoMn2O4的多孔空心球结构。首先,采用溶剂热法合成了不同比例金属离子的碳酸盐,形貌均匀,尺寸均一；一定温度下煅烧,由于两种金属离子不同的扩散速率,柯肯达尔效应原理,形成空心球状结构。MnCO2O4具有立方结构,而CoMn2O4是四方结构。初步的电化学性能测试结果显示在电流密度200mA/g下进行充放电测试,立方相的MnCo2O4首次容量为1473mAh/g,循环10次后为978mAh/g,而CoMn2O4首次容量为1357mAh/g,循环10次后为809mAh/g,显示出了潜在的应用价值。
In this dissertation, controlled synthesis and properties were developed to prepare bismuthoxychloride and manganese-based compounds with porous structures. Regular3D BiOC1microstructutes were synthesized solvothermally and porous MnO2microplates and microspheres, MnCo2O4and CoMnO4hollow microspheres were produced through hydro-/solvo-thermal methods followed by the pyrolysis of the precursors. The electrochemical hydrogen storage properties of BiOC1microstructures were investigated in Ni/H battery model. We also study the behaviors of manganese-based compounds as anode in a rechargeable lithium battery. The main points are summarized as follows:
1. Several3D BiOC1microstructures, such as2500nm peonies,1000nm ball-flowers, and3000nm rough spheres are selectively and solvothermally prepared. These microstructures are composed of nanoplate with size of～1000nm,～300nm and～200nm, respectively, the growth surface of which are all (001). Based on the results of the time-depended experiments, we propose the possible forming mechanism as "fast nucleation-oriented attachment-fusion". N2adsorption desorption isotherms demonstrate that the rough spheres possesse the largest special surface area and pore volume, which affect the electrochemical hydrogen storage behavior. Electrochemical tests indicate that the sample with the larger special surface area and pore volume possesses the higher storage capacity of hydrogen. We assumed that hydrogen entered into the interlayer between (001) facets considerring its largest interplanar spacing. In addition, the hydrogen storage study of BiOCl microspheres composed of nanoplates with exposed facet perpendicular to [2(-)21] axis indicates that hydrogen enters into the interlayer. The above results of research have been in press in the international jounal of Journal of Nanoscience and Nanotechnology.
2. MnCO3microstructures, including microplates with the average diameter of2.3μm and thickness of about200nm and microspheres with the average diameter of3.1μm stacked with50nm-thick sheets, were hydrothermally prepared in the presence of sodium dodecyl benzene sulphonate (SDBS) and dodecyl sulfonic acid sodium (SDS), respectively. With the as-synthesized MnCO3as precursors followed by annealing at400℃for4h, porous γ-MnO2microplates and microspheres with different pore sizes, which basically remained the initial shapes, were obtained. The former with the narrower pore size diameter and the larger special surface area performs a better behavior for lithium battery. The electrochemical property tests over Li+batteries showed that the initial discharge capacity of the as-prepared γ-MnO2microplates and microspheres were1997mAh·-g-1and1533mAh·g-1. Noticeably, even after100cycles, the discharge capacity of γ-MnO2microplates was still as high as626mAh·g-1, showing the decent cycle behavior. The above results of research have been published in the international jounal of Journal of Alloys and Compounds.
3. Porous MnCo2O4and CoMn2O4hollow microspheres were synthesized through the pyrolysis of carbonates, which were obtained solvothermally by tuning the ratio of Mn/Co. Firstly, relatively uniform carbonate microspheres with different components were solvothermally produced; after calcining at a centain temperature, porous hollow microspheres were obtained due to the different diffusion rate of the two metal ions (Kirkendall effect). The X-ray diffraction patterns indicate that MnCo2O4is cubic phase, whereas CoMn2O4is a tetragonal structure. The preliminary electrochemical property tests over Li+batteries showed that the initial discharge capacity of the as-prepared MnCo2O4and COMn2O4hollow microspheres were1473mAh·g-1and1357mAh·g-1. After10cycles, the discharge capacity of the MnCo2O4and CoMn2O4hollow microspheres were978and809mAh-g"1, respectively, indicating their potential application in lithium battery.
1、采用溶剂热法选择性合成了3D的BiOCl微米结构,如2.5μm的牡丹花状,1μm的球花状和3μm的粗糙球状结构。这些结构分别由直径1000nm,300nm,200nm的片堆积而成,表征发现片的生长面均是(001)。基于不同反应时间的产品表征结果,我们提出了“快速成核-定向排列-边界融合”的生长过程。N2吸附脱附曲线表明粗糙球结构具有最大的比表面积数据和孔体积数据,这影响其电化学储氢的性能。电化学储氢测试表明有较大比表面和孔体积的样品具有更大的储氢容量值。考虑到其(001)面较大的层间距,我们推测(001)面的层间空隙储存活性H。此外,我们还研究了生长面为[2(-)21]法向的纳米片堆积而成的微米球结构,结果进一步证实了活性H进入了BiOCl的层间。相关实验结果发表在杂志Journal of Nanoscience and Nanotechnology上。
2、分别在表面活性剂十二烷基苯磺酸钠(SDBS)和十二烷基磺酸钠(SDS)的辅助下,直径2.3μm厚度200nm的均匀微米片和由厚度50nm的纳米片堆积而成的直径3.1μm的花状球结构的MnCO3,在水热条件下合成出来。合成的MnCO3经400℃煅烧4小时,我们得到了多孔的的y-MnO2片状和花球状结构。前者具有更窄的孔径分布以及更大的比表面积,更利于Li+的存储和传输,而表现出了优良的储锂性能。测试结果显示在100mA/g的电流密度下两种结构的首次放电容量分别为1997mAh/g和1533mAh/g。值得指出的是,γ-MnO2多孔片状结构经100次循环后,其容量仍然保持在626mAh/g,呈现了较优良的循环性能。该项研究成果发表在Journal of Alloys and Compounds上。
3、通过控制反应物Mn/Co的摩尔比,利用热解碳酸盐前驱体的方法,选择性合成了MnCO2O4和CoMn2O4的多孔空心球结构。首先,采用溶剂热法合成了不同比例金属离子的碳酸盐,形貌均匀,尺寸均一；一定温度下煅烧,由于两种金属离子不同的扩散速率,柯肯达尔效应原理,形成空心球状结构。MnCO2O4具有立方结构,而CoMn2O4是四方结构。初步的电化学性能测试结果显示在电流密度200mA/g下进行充放电测试,立方相的MnCo2O4首次容量为1473mAh/g,循环10次后为978mAh/g,而CoMn2O4首次容量为1357mAh/g,循环10次后为809mAh/g,显示出了潜在的应用价值。
In this dissertation, controlled synthesis and properties were developed to prepare bismuthoxychloride and manganese-based compounds with porous structures. Regular3D BiOC1microstructutes were synthesized solvothermally and porous MnO2microplates and microspheres, MnCo2O4and CoMnO4hollow microspheres were produced through hydro-/solvo-thermal methods followed by the pyrolysis of the precursors. The electrochemical hydrogen storage properties of BiOC1microstructures were investigated in Ni/H battery model. We also study the behaviors of manganese-based compounds as anode in a rechargeable lithium battery. The main points are summarized as follows:
1. Several3D BiOC1microstructures, such as2500nm peonies,1000nm ball-flowers, and3000nm rough spheres are selectively and solvothermally prepared. These microstructures are composed of nanoplate with size of～1000nm,～300nm and～200nm, respectively, the growth surface of which are all (001). Based on the results of the time-depended experiments, we propose the possible forming mechanism as "fast nucleation-oriented attachment-fusion". N2adsorption desorption isotherms demonstrate that the rough spheres possesse the largest special surface area and pore volume, which affect the electrochemical hydrogen storage behavior. Electrochemical tests indicate that the sample with the larger special surface area and pore volume possesses the higher storage capacity of hydrogen. We assumed that hydrogen entered into the interlayer between (001) facets considerring its largest interplanar spacing. In addition, the hydrogen storage study of BiOCl microspheres composed of nanoplates with exposed facet perpendicular to [2(-)21] axis indicates that hydrogen enters into the interlayer. The above results of research have been in press in the international jounal of Journal of Nanoscience and Nanotechnology.
2. MnCO3microstructures, including microplates with the average diameter of2.3μm and thickness of about200nm and microspheres with the average diameter of3.1μm stacked with50nm-thick sheets, were hydrothermally prepared in the presence of sodium dodecyl benzene sulphonate (SDBS) and dodecyl sulfonic acid sodium (SDS), respectively. With the as-synthesized MnCO3as precursors followed by annealing at400℃for4h, porous γ-MnO2microplates and microspheres with different pore sizes, which basically remained the initial shapes, were obtained. The former with the narrower pore size diameter and the larger special surface area performs a better behavior for lithium battery. The electrochemical property tests over Li+batteries showed that the initial discharge capacity of the as-prepared γ-MnO2microplates and microspheres were1997mAh·-g-1and1533mAh·g-1. Noticeably, even after100cycles, the discharge capacity of γ-MnO2microplates was still as high as626mAh·g-1, showing the decent cycle behavior. The above results of research have been published in the international jounal of Journal of Alloys and Compounds.
3. Porous MnCo2O4and CoMn2O4hollow microspheres were synthesized through the pyrolysis of carbonates, which were obtained solvothermally by tuning the ratio of Mn/Co. Firstly, relatively uniform carbonate microspheres with different components were solvothermally produced; after calcining at a centain temperature, porous hollow microspheres were obtained due to the different diffusion rate of the two metal ions (Kirkendall effect). The X-ray diffraction patterns indicate that MnCo2O4is cubic phase, whereas CoMn2O4is a tetragonal structure. The preliminary electrochemical property tests over Li+batteries showed that the initial discharge capacity of the as-prepared MnCo2O4and COMn2O4hollow microspheres were1473mAh·g-1and1357mAh·g-1. After10cycles, the discharge capacity of the MnCo2O4and CoMn2O4hollow microspheres were978and809mAh-g"1, respectively, indicating their potential application in lithium battery.
引文
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