混合过渡金属氧化物纳米材料的制备及其锂离子电池性能的研究
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摘要
近些年来,纳米尺度的金属化物由于齐相对于石墨能够提供较高的可逆容量(600-1000mAh/g)和能量密度,被广泛认为是一种具有应用潜力的锂离子电池电极材料。这些金属氧化物与锂的反应机制不同于传统的品格嵌入/脱出机制；一般金属氧化物有两种储锂机制：第一类是通过与锂离子的合金/脱合金过程储锂;另外一类则是通过相的转换即金属的还原/氧化过程储锂。属于第一类的典型的金属氧化物为Sn、Zn、In和Sb的氧化物;以Sn02为例,其储锂机制包含SnO2+4Li→Sn+2Li2O和mSn+nLi(?)LinSnm两步反应。而属于第二类的金属氧化物包括Co3O4,NiO,Fe2O3等多数过渡金属氧化物;这一类氧化物通过与Li发生氧化还原反应进行储锂;在放电过程中氧化物被还原为金属单质,而Li则形成无定型的Li2O；此后的循环过程中主要为金属的氧化/还原和Li2O的分解和生成过程。因此,此类氧化物的理论容量取决于参与反应的过渡金属氧化物的氧化态。这类转换反应机制的电极反应式可以被概括为MxO+2Li++2e-→←xM0+Li20。
但是,金属氧化物自身也存在一定的缺陷从而限制了其应用。比如首次循环不可逆容量过高造成锂离子的损失,较大的塑性形变导致的不可逆容量损失严重,致使其循环稳定性较差等等。针对上述问题,无数科学家对过渡金属氧化物改性方面做了大量工作,比如将氧化物进行纳米化、与碳或者石墨烯进行复合、对氧化物进行贵金属掺杂以提高其导电性等等。最近,期望合成混合过渡金属氧化物,利用两种甚至多种金属的协同储锂和改良活性来提升电极材料性能成为了一种新的受关注的手段。本文中,我们制备了ZnFe2O4、CuFe2O4和MnWO4双金属混合氧化物,来研究其中两种金属的相互作用及其对于电化学性能的提升效果。
我们以乙酸锌和硫酸亚铁为原料利用一步水热合成方法制备得到了平均粒径约为200nm左右规则的ZnFe2O4八面体纳米颗粒。通过XRD,SEM和HRTEM的分析可以确定,ZnFe2O4(?)内米颗粒的八个面均由{111}晶面闱绕。ZnFe2O4八面体纳米颗粒表现出了优良的电化学性能。在60mA·g-1小电流下,循环80圈以后电池的可逆容量仍然高达910mAh·g-1;其倍率性能以及在大电流下的循环性能也同样出色,1000mA·g-1的大电流下循环300圈以后容量仍然能够保持在730mAh·g-1以上。我们利用非原位HRTEM和SAED对于若干次循环以后的完全充电和放电的电极材料进行了深入分析,发现八面体颗粒在充放电以后发生了巨大的结构重组和形变,内部外部结构都发生了变化；此外我门还结合循环伏安和充放电曲线给出了ZnFe2O4作为电极材料时可能的电极反应
我们利用简单的一步高温固相反应以草酸铁和乙酸铜为原料选择性合成了具有不同结构和粒径的CuFe2O4纳米颗粒。其中400℃合成的立方相CuFe2O4(c-CuFe2O4400)平均粒径约为50-100nm,800℃合成的立方相CuFe2O4(c-CuFe2O4800)和四方相CuFe2O4(t-CuFe2O4)平均粒径约为800nm左右。我们对比了不同结构CuFe2O4的电化学反应机理,发现两相CuFe2O4的电极反应只有首次放电时表现不同,其中c-CuFe2O4在首次循环时会生成LixCuFe2O4(?)中间状态,而t-CuFe2O4则观察不到这种晶格嵌锂的现象。此外,c-CuFe2O4(400)作为电极材料的电化学性能最为出色,100mA·g-1的电流密度下循环60圈容量仍然能够保持于950mAh·g-1以上;此外,其倍率性能也十分优秀,5000mA·g-1的电流密度下结构仍然能够保持稳定。我们还首次通过非原位HRTEM的分析发现了CuFe2O4的放电产物中不仅有单质Cu和Fe的存在,还有FexCu1-x亚稳相合金结构的存在,这也部分解释了金属Cu加入氧化铁中对于体系的电化学稳定性提高的原因。
我们还利用一步水热合成方法制备得到了具有密集空洞结构的MnWO4纳米颗粒,样品由大量的颗粒尺寸为20-30nm形貌均一的纳米颗粒组成;颗粒内部的纳米孔洞大小约为5-8nm。MnWO4纳米颗粒的电化学性能优异,其在100mA·g-1的电流密度下循环160圈以后容量仍然保持在600mAh-g"1以上,远高于已经报道类似结构的负极材料。这种独特的内部空洞几何结构可能对于提高其循环能力有着至关重要的作用。
我们的这些工作为制备混合过渡金属氧化物纳米材料提供了简便可行的方法,并且为这一类有应用潜质的、长寿命高性能锂离子电极材料的实际应用提供了一种可能性。
Metal oxides have long been considered as promising anode materials for lithium-ion batteries (LIB) to improve the graphite anode, because they could gain much higher specific capacity and power density compared with the graphite-based anode. The metal oxides reactions with Li do not via the classical insertion/deinsertion process:the reactions involve in two different mechanisms:one type is based on a Li-alloying/dealloying process; another type involves a displacive phase transition. The typical materials of the first type are Sn, Zn, In and Sb oxides; the oxides irreversibly deoxidized to metal, then the metal could reversibly alloy with lithium to uptake one or more lithium per metal atom. Take SnO2for instance, the reactions routes are SnO2+4Li→Sn+2Li2O, and mSn+nLi(?)LinSnm. The oxides of the second type include Co3O4, NiO, Fe2O3and so on; the reaction process with Li contains the reversibly reduction of the oxide, then the formation and decomposition of Li2O matrix, along with the reduction and oxidation of metal. These oxides could achieve quite high reversible capacity due to the multi-electron redox process; in this case, the specific capacity depends on the oxidation state of the transition metal participate in the reaction. The general equation of conversion reaction is described as MxO+2Li++2e-(?)xM0+Li2O.
However, there are several drawbacks preventing the transitional-based anodes from being commercial uses, such as the low energy efficiency during the first discharge process large volume changes and poor capacity retention. To overcome these obstacles, intensive researches like tailoring metal oxides materials to the nanoscale, forming nanocomposites with carbon materials and graphene, and doping with novel metal particles have been conducted. Recently, fabricating nanosized mixed metal oxide compounds with superior capability becomes a new strategy to improve the performance. In this paper, we fabricated binary metal oxides like ZnFe2O4, CuFe2O4and Mn WO4to research their electrochemical performance.
Regular ZnFe2O4octahedrons with an average size of200nm have been synthesized through a one step hydrothermal method by zinc acetate and ferrous chloride. XRD, SEM and HRTEM studies reveal that the products are highly crystallized and uniformly enclosed by{111} facet. Galvanostatic cycling lithium battery anode at60mA·g-1between0.01and3.0V up to80cycles exhibits a high capacity of910mAh·g-1. The ZnFeO4octahedrons also exhibit an excellent rate performance, and deliver stable reversible specific capacity of730inAh·g-1even after300cycles at1000mA·g-1. The reaction mechanism for Li-recyclability is proposed based on the ex-situ HRTEM and SAED analysis of the electrodes after completely discharged and charged together with voltage profile and cyclic voltammetry. The lithium-driven structural reorganization and plasticity deformation of electrode materials are observed and discussed specifically.
Cubic CuFe2O4(c-CuFe2O4and tetragonal CuFe2O4(t-CuFe2O4) nanoparticles were selectively prepared using a facile one-step solid state reaction route by ferrous oxalate and copper acetate as the reactants. As an anode material for Li-ion batteries, the electrode reactions of the two phases CuFe2O4are similar except the lithium insertion process during the first discharge; the preceding Lithium intercalation occurred and formed intermediate phase LixCuFe2O4when c-CuFe2O4was applied as anode material, but this intermediate phase is hardly observed in the t-CuFe2O4. Compared with c-CuFe2O4and t-CuFe2O4synthesized at800℃, c-CuFe2O4synthesized at400℃with larger surface area exhibited superior discharge capacities with good cycling performance (950mAh·g-1at100mA·g-1after60cycles), and higher rate capability. Through ex-situ HRTEM analysis, we observed the existence of metastable FexCu1-x alloy in the discharged nanocomposition for the first time, which exhibits the interaction of metallic Cu particles with the adjacent iron ions.
The MnWO4nanobars with dense nanocavities have been synthesized through hydrothermal route; the average particle size of the MnW04nanobars is about20-30nm, and the nanocavities inside are about5-8nm. Galvanostatic cycling of MnWO4lithium battery anode exhibit an excellent rate performance. The improved electrochemical performance could be attributed to the unique geometry nanocavities and improved accommodation of the transformation strains during cycling.
These works resulted in convenient methods for obtaining mixed metal oxide nanomaterials, and provided an opportunity to further application of these promising materials with the remarkable performance, both in terms of long life span and rate capability.
但是,金属氧化物自身也存在一定的缺陷从而限制了其应用。比如首次循环不可逆容量过高造成锂离子的损失,较大的塑性形变导致的不可逆容量损失严重,致使其循环稳定性较差等等。针对上述问题,无数科学家对过渡金属氧化物改性方面做了大量工作,比如将氧化物进行纳米化、与碳或者石墨烯进行复合、对氧化物进行贵金属掺杂以提高其导电性等等。最近,期望合成混合过渡金属氧化物,利用两种甚至多种金属的协同储锂和改良活性来提升电极材料性能成为了一种新的受关注的手段。本文中,我们制备了ZnFe2O4、CuFe2O4和MnWO4双金属混合氧化物,来研究其中两种金属的相互作用及其对于电化学性能的提升效果。
我们以乙酸锌和硫酸亚铁为原料利用一步水热合成方法制备得到了平均粒径约为200nm左右规则的ZnFe2O4八面体纳米颗粒。通过XRD,SEM和HRTEM的分析可以确定,ZnFe2O4(?)内米颗粒的八个面均由{111}晶面闱绕。ZnFe2O4八面体纳米颗粒表现出了优良的电化学性能。在60mA·g-1小电流下,循环80圈以后电池的可逆容量仍然高达910mAh·g-1;其倍率性能以及在大电流下的循环性能也同样出色,1000mA·g-1的大电流下循环300圈以后容量仍然能够保持在730mAh·g-1以上。我们利用非原位HRTEM和SAED对于若干次循环以后的完全充电和放电的电极材料进行了深入分析,发现八面体颗粒在充放电以后发生了巨大的结构重组和形变,内部外部结构都发生了变化；此外我门还结合循环伏安和充放电曲线给出了ZnFe2O4作为电极材料时可能的电极反应
我们利用简单的一步高温固相反应以草酸铁和乙酸铜为原料选择性合成了具有不同结构和粒径的CuFe2O4纳米颗粒。其中400℃合成的立方相CuFe2O4(c-CuFe2O4400)平均粒径约为50-100nm,800℃合成的立方相CuFe2O4(c-CuFe2O4800)和四方相CuFe2O4(t-CuFe2O4)平均粒径约为800nm左右。我们对比了不同结构CuFe2O4的电化学反应机理,发现两相CuFe2O4的电极反应只有首次放电时表现不同,其中c-CuFe2O4在首次循环时会生成LixCuFe2O4(?)中间状态,而t-CuFe2O4则观察不到这种晶格嵌锂的现象。此外,c-CuFe2O4(400)作为电极材料的电化学性能最为出色,100mA·g-1的电流密度下循环60圈容量仍然能够保持于950mAh·g-1以上;此外,其倍率性能也十分优秀,5000mA·g-1的电流密度下结构仍然能够保持稳定。我们还首次通过非原位HRTEM的分析发现了CuFe2O4的放电产物中不仅有单质Cu和Fe的存在,还有FexCu1-x亚稳相合金结构的存在,这也部分解释了金属Cu加入氧化铁中对于体系的电化学稳定性提高的原因。
我们还利用一步水热合成方法制备得到了具有密集空洞结构的MnWO4纳米颗粒,样品由大量的颗粒尺寸为20-30nm形貌均一的纳米颗粒组成;颗粒内部的纳米孔洞大小约为5-8nm。MnWO4纳米颗粒的电化学性能优异,其在100mA·g-1的电流密度下循环160圈以后容量仍然保持在600mAh-g"1以上,远高于已经报道类似结构的负极材料。这种独特的内部空洞几何结构可能对于提高其循环能力有着至关重要的作用。
我们的这些工作为制备混合过渡金属氧化物纳米材料提供了简便可行的方法,并且为这一类有应用潜质的、长寿命高性能锂离子电极材料的实际应用提供了一种可能性。
Metal oxides have long been considered as promising anode materials for lithium-ion batteries (LIB) to improve the graphite anode, because they could gain much higher specific capacity and power density compared with the graphite-based anode. The metal oxides reactions with Li do not via the classical insertion/deinsertion process:the reactions involve in two different mechanisms:one type is based on a Li-alloying/dealloying process; another type involves a displacive phase transition. The typical materials of the first type are Sn, Zn, In and Sb oxides; the oxides irreversibly deoxidized to metal, then the metal could reversibly alloy with lithium to uptake one or more lithium per metal atom. Take SnO2for instance, the reactions routes are SnO2+4Li→Sn+2Li2O, and mSn+nLi(?)LinSnm. The oxides of the second type include Co3O4, NiO, Fe2O3and so on; the reaction process with Li contains the reversibly reduction of the oxide, then the formation and decomposition of Li2O matrix, along with the reduction and oxidation of metal. These oxides could achieve quite high reversible capacity due to the multi-electron redox process; in this case, the specific capacity depends on the oxidation state of the transition metal participate in the reaction. The general equation of conversion reaction is described as MxO+2Li++2e-(?)xM0+Li2O.
However, there are several drawbacks preventing the transitional-based anodes from being commercial uses, such as the low energy efficiency during the first discharge process large volume changes and poor capacity retention. To overcome these obstacles, intensive researches like tailoring metal oxides materials to the nanoscale, forming nanocomposites with carbon materials and graphene, and doping with novel metal particles have been conducted. Recently, fabricating nanosized mixed metal oxide compounds with superior capability becomes a new strategy to improve the performance. In this paper, we fabricated binary metal oxides like ZnFe2O4, CuFe2O4and Mn WO4to research their electrochemical performance.
Regular ZnFe2O4octahedrons with an average size of200nm have been synthesized through a one step hydrothermal method by zinc acetate and ferrous chloride. XRD, SEM and HRTEM studies reveal that the products are highly crystallized and uniformly enclosed by{111} facet. Galvanostatic cycling lithium battery anode at60mA·g-1between0.01and3.0V up to80cycles exhibits a high capacity of910mAh·g-1. The ZnFeO4octahedrons also exhibit an excellent rate performance, and deliver stable reversible specific capacity of730inAh·g-1even after300cycles at1000mA·g-1. The reaction mechanism for Li-recyclability is proposed based on the ex-situ HRTEM and SAED analysis of the electrodes after completely discharged and charged together with voltage profile and cyclic voltammetry. The lithium-driven structural reorganization and plasticity deformation of electrode materials are observed and discussed specifically.
Cubic CuFe2O4(c-CuFe2O4and tetragonal CuFe2O4(t-CuFe2O4) nanoparticles were selectively prepared using a facile one-step solid state reaction route by ferrous oxalate and copper acetate as the reactants. As an anode material for Li-ion batteries, the electrode reactions of the two phases CuFe2O4are similar except the lithium insertion process during the first discharge; the preceding Lithium intercalation occurred and formed intermediate phase LixCuFe2O4when c-CuFe2O4was applied as anode material, but this intermediate phase is hardly observed in the t-CuFe2O4. Compared with c-CuFe2O4and t-CuFe2O4synthesized at800℃, c-CuFe2O4synthesized at400℃with larger surface area exhibited superior discharge capacities with good cycling performance (950mAh·g-1at100mA·g-1after60cycles), and higher rate capability. Through ex-situ HRTEM analysis, we observed the existence of metastable FexCu1-x alloy in the discharged nanocomposition for the first time, which exhibits the interaction of metallic Cu particles with the adjacent iron ions.
The MnWO4nanobars with dense nanocavities have been synthesized through hydrothermal route; the average particle size of the MnW04nanobars is about20-30nm, and the nanocavities inside are about5-8nm. Galvanostatic cycling of MnWO4lithium battery anode exhibit an excellent rate performance. The improved electrochemical performance could be attributed to the unique geometry nanocavities and improved accommodation of the transformation strains during cycling.
These works resulted in convenient methods for obtaining mixed metal oxide nanomaterials, and provided an opportunity to further application of these promising materials with the remarkable performance, both in terms of long life span and rate capability.
引文
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