锰基电极材料的微纳化合成、表征与电化学性能研究
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摘要
论文发展了水热法在硼砂辅助下,不使用表活剂和模版一步合成了Mn3O4超细一维纳米线;利用水镁石晶体结构的生长习性,一步水热法合成了Mn(OH)2六角片,结合CVD法在乙炔气氛中,控制制备了一系列MnO@C核壳纳米片;在乙二醇-水-水合肼组成的三元混合溶剂热体系中,控制合成了一系列Mn(OH)2等级结构,结合高温固相法,控制制各了一系列Mn2O3多孔等级结构：室温水相一步合成Mn3O4八面体。本论文的主要内容归纳如下：
1.采用一步水热法,不使用任何表活剂或模版,通过硼砂的辅助作用,在200℃反应15h,合成了直径大约为15nm长度为微米级的Mn3O4一维超细纳米线,通过时间对比实验研究了纳米线的生长过程,是由非晶纳米线晶化和由短变长的Ostwald熟化过程,在5K时,Mn3O4(?)纳米线的矫顽力为5600Oe。Mn3O4纳米线作为前驱与锂源混合通过高温固相反应,在750℃反应6h,制备了LiMn2O4致密多面体,在0.1倍率充放60次,比容量达到115mA h g-1保持率为98.3%.相关研究成果发表在CrystEngComm杂志上。
2.采用水热法,利用水镁石矿结构的晶体生长习性,在180℃反应12h,一步合成了Mn(OH)2纳米片,将Mn(OH)2纳米片在乙炔气氛围下热处理,得到了尺寸约为150nm的MnO@C核壳纳米片,通过控制热处理时间和反应温度,碳层的厚度大约可控制在3.1到13.7nm的范围内。电化学性能测试结果显示,在550℃反应10h合成的MnO@C纳米片碳层厚度约为8.1nm,在200mA g-1电流密度下,放电比容量高达770mA h g-1和展示出良好的稳定性能,且比容量高于碳层厚度约为3.1,4.0,4.2,10.9和13.7nm的核壳纳米片。相关研究部分成果发表在J. Mater.Chem.(?)杂志上。
3.采用乙二醇-水-水合肼组成的二元混合溶剂热体系中,在180℃反应12h,通过改变乙二醇与水的体积比,我们得到了系列Mn(OH)2等级结构,例如：纳米片组成的花状结构、纳米片组成的片状结构、部分纳米片脱离的片状结构和纳米片。值得指出的是,这些纳米片具有不同的厚度。通过在空气中600℃热处理12h前驱物Mn(OH)2,我们得到了Mn2O3多孔等级结构。电化学性能测试Mn2O3的系列样品发现,由纳米片堆积而成的多孔花状具有高的比容量和循环稳定性。在300mA g-1电流密度下,100次充放电后,比容量大约为521mA h g-1较薄的厚度和表面的多孔结构是有利于其电化学性能改善和提高。
4.室温条件水相中,使用草酸铵辅助,利用四方晶系的生长习性,合成Mn3O4八面体,研究Mn3O4八面体的生长机制、磁性及电化学性能。
In this paper, hydrothermal method was developed to synthesis Mn3O4nanowires with the assistance of sodium borate and without any surfactants or templates; Using the inherent crystal tendency of brucite crystal, combined with the CVD method in acetylene atmosphere, synthesis of a series of MnO@C core-shell nanoplates; In ethylene glycol-water-hydrazine hydrate ternary mixed solvent system, control the synthesis of a series of Mn(OH)2hierarchical structures, combined with solid state method, obtained a series of Mn2O3hierarchical structures. Mn3O4octahedrons were synthesis in water phase at room temperature. The main contents are summarized as follows:
1. With the assistance of sodium borate, the Mn3O4nanowires with diameter of-15nm and a length of up to several micrometres have been hydrothermally synthesized at200℃for15h without any surfactants or templates. It was investigated that during the formation process of Mn3O4nanowires the length of the nanowires increased while the diameter did not obviously change, it could be believed that the formation of Mn3O4nanowires followed the Ostwald ripening process. The coercivity of the Mn3O4nanowires is up to5600Oe at5K. As these Mn3O4nanowires were treated with LiOH by solid state reaction at750℃for6h, interconnected LiMn2O4polyhedrons were obtained. The achieved discharge capacity of the LiMn2O4polyhedrons was115mA h g-1and they retained98.3%of this capacity after60cycles at0.1C. The above results of research have been published in CrystEngComm.
2. Using the inherent crystal tendency of brucite crystal, Mn(OH)2nanoplates with size of-150nm have been hydrothermally synthesized at180℃for12h. MnO@C core-shell nanoplates with a size of-150nm have been prepared via thermal treatment deposition of acetylene with the precursor of Mn(OH)2nanoplates. The thickness of the carbon shells varied from-3.1to13.7nm by controlling the treatment temperature and reaction duration time. The electrochemical performance of the MnO@C nanoplates, which were synthesized at550℃for10h with a carbon shell thickness of-8.1nm, display a high reversible capacity of-770mA h g-1at a current density of200mA g-1and good cyclability after prolonged testing, which is higher than that of MnO@C nanoplates with a carbon shell thickness of～3.1,4.0,4.2,10.9and13.7nm. The above results of research have been published in J. Mater. Chem.
3. Mn(OH)2hierarchical structures were obtained in the ethylene glycol-water-hydrazine hydrate system with different ethylene glycol/water volume ratio. Such as, nanosheets stacking flower structure, nanoplates stacking plate structure, partial fallen stacking plate structure and nanplate. It should be point out that the nanosheet and nanoplates own different thickness.Mn2O3porous hierarchical structures have been fabricated from the Mn(OH)2precursor in air atmosphere at600℃for12h. When these Mn2O3samples used as anode materials for lithium-ion batteries, the Mn2O3porous stacking nanosheets displays a high and stable reversible capacity of～521mA h g-1at a current density of300mA g-1after100cycles. The compared experiments indicate that both thin thickness of nanosheets and porous structure of the Mn2O3are favorable for electrodes of lithium-ion batteries with improved specific capacity and rate performance.
4. With the assistance of ammonium oxalate, the Mn3O4octahedrons have been synthesised at room temperature by using the inherent crystal tendency. It investigates the information mechanism, magnetism and electrochemical performances of Mn3O4octahedrons.
1.采用一步水热法,不使用任何表活剂或模版,通过硼砂的辅助作用,在200℃反应15h,合成了直径大约为15nm长度为微米级的Mn3O4一维超细纳米线,通过时间对比实验研究了纳米线的生长过程,是由非晶纳米线晶化和由短变长的Ostwald熟化过程,在5K时,Mn3O4(?)纳米线的矫顽力为5600Oe。Mn3O4纳米线作为前驱与锂源混合通过高温固相反应,在750℃反应6h,制备了LiMn2O4致密多面体,在0.1倍率充放60次,比容量达到115mA h g-1保持率为98.3%.相关研究成果发表在CrystEngComm杂志上。
2.采用水热法,利用水镁石矿结构的晶体生长习性,在180℃反应12h,一步合成了Mn(OH)2纳米片,将Mn(OH)2纳米片在乙炔气氛围下热处理,得到了尺寸约为150nm的MnO@C核壳纳米片,通过控制热处理时间和反应温度,碳层的厚度大约可控制在3.1到13.7nm的范围内。电化学性能测试结果显示,在550℃反应10h合成的MnO@C纳米片碳层厚度约为8.1nm,在200mA g-1电流密度下,放电比容量高达770mA h g-1和展示出良好的稳定性能,且比容量高于碳层厚度约为3.1,4.0,4.2,10.9和13.7nm的核壳纳米片。相关研究部分成果发表在J. Mater.Chem.(?)杂志上。
3.采用乙二醇-水-水合肼组成的二元混合溶剂热体系中,在180℃反应12h,通过改变乙二醇与水的体积比,我们得到了系列Mn(OH)2等级结构,例如：纳米片组成的花状结构、纳米片组成的片状结构、部分纳米片脱离的片状结构和纳米片。值得指出的是,这些纳米片具有不同的厚度。通过在空气中600℃热处理12h前驱物Mn(OH)2,我们得到了Mn2O3多孔等级结构。电化学性能测试Mn2O3的系列样品发现,由纳米片堆积而成的多孔花状具有高的比容量和循环稳定性。在300mA g-1电流密度下,100次充放电后,比容量大约为521mA h g-1较薄的厚度和表面的多孔结构是有利于其电化学性能改善和提高。
4.室温条件水相中,使用草酸铵辅助,利用四方晶系的生长习性,合成Mn3O4八面体,研究Mn3O4八面体的生长机制、磁性及电化学性能。
In this paper, hydrothermal method was developed to synthesis Mn3O4nanowires with the assistance of sodium borate and without any surfactants or templates; Using the inherent crystal tendency of brucite crystal, combined with the CVD method in acetylene atmosphere, synthesis of a series of MnO@C core-shell nanoplates; In ethylene glycol-water-hydrazine hydrate ternary mixed solvent system, control the synthesis of a series of Mn(OH)2hierarchical structures, combined with solid state method, obtained a series of Mn2O3hierarchical structures. Mn3O4octahedrons were synthesis in water phase at room temperature. The main contents are summarized as follows:
1. With the assistance of sodium borate, the Mn3O4nanowires with diameter of-15nm and a length of up to several micrometres have been hydrothermally synthesized at200℃for15h without any surfactants or templates. It was investigated that during the formation process of Mn3O4nanowires the length of the nanowires increased while the diameter did not obviously change, it could be believed that the formation of Mn3O4nanowires followed the Ostwald ripening process. The coercivity of the Mn3O4nanowires is up to5600Oe at5K. As these Mn3O4nanowires were treated with LiOH by solid state reaction at750℃for6h, interconnected LiMn2O4polyhedrons were obtained. The achieved discharge capacity of the LiMn2O4polyhedrons was115mA h g-1and they retained98.3%of this capacity after60cycles at0.1C. The above results of research have been published in CrystEngComm.
2. Using the inherent crystal tendency of brucite crystal, Mn(OH)2nanoplates with size of-150nm have been hydrothermally synthesized at180℃for12h. MnO@C core-shell nanoplates with a size of-150nm have been prepared via thermal treatment deposition of acetylene with the precursor of Mn(OH)2nanoplates. The thickness of the carbon shells varied from-3.1to13.7nm by controlling the treatment temperature and reaction duration time. The electrochemical performance of the MnO@C nanoplates, which were synthesized at550℃for10h with a carbon shell thickness of-8.1nm, display a high reversible capacity of-770mA h g-1at a current density of200mA g-1and good cyclability after prolonged testing, which is higher than that of MnO@C nanoplates with a carbon shell thickness of～3.1,4.0,4.2,10.9and13.7nm. The above results of research have been published in J. Mater. Chem.
3. Mn(OH)2hierarchical structures were obtained in the ethylene glycol-water-hydrazine hydrate system with different ethylene glycol/water volume ratio. Such as, nanosheets stacking flower structure, nanoplates stacking plate structure, partial fallen stacking plate structure and nanplate. It should be point out that the nanosheet and nanoplates own different thickness.Mn2O3porous hierarchical structures have been fabricated from the Mn(OH)2precursor in air atmosphere at600℃for12h. When these Mn2O3samples used as anode materials for lithium-ion batteries, the Mn2O3porous stacking nanosheets displays a high and stable reversible capacity of～521mA h g-1at a current density of300mA g-1after100cycles. The compared experiments indicate that both thin thickness of nanosheets and porous structure of the Mn2O3are favorable for electrodes of lithium-ion batteries with improved specific capacity and rate performance.
4. With the assistance of ammonium oxalate, the Mn3O4octahedrons have been synthesised at room temperature by using the inherent crystal tendency. It investigates the information mechanism, magnetism and electrochemical performances of Mn3O4octahedrons.
引文
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