LiMVO_4（M=Cu，Ni，Mn）型锂离子电池材料的高压结构研究
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摘要
在当今社会，解决能源紧张问题已刻不容援。锂离子电池的发展也因此受到了广泛关注。在锂离子正负极性能的比较中，负极选用的碳材料的技术标准无论是在理论和实际应用上都已经非常成熟，而正极材料的选择还具有很大提高空间。最近，GT-K.Fey等人最先合成了尖晶石结构的LiNiVO_4,其锂离子的脱嵌电压可以达到4.8V，开创了5V锂离子电池正极材料的先河。自此具有尖晶石结构的一类锂离子电池正极材料进入了科研工作者的研究视野。本论文选取了3种具有代表性的当今热点聚阴锂离子电池正极材料LiMVO_4(M=Cu, Ni, Mn)。该类三元金属酸盐氧化物材料都具有反尖晶石结构，但是各自具有不同的结构对称性。首先，被广泛关注的材料LiCuVO_4,其并不仅仅是5V正极材料，由于其正交的反尖晶石结构中Cu-O-Cu特殊的成键性质以及原包结构内部的层状原子排布，使得其也备受磁学方面的关注。我们同样选取了LiCuVO_4在常压下具有正交的反尖晶石结构的样品，对其进行了原位高压Raman光谱的实验，发现其在20GPa时Raman峰部分消失，并且伴随新峰的出现。并且峰位也不同程度的发生了畸变。由此我们可以断定其发生了结构相变。同步辐射XRD研究显示其20GPa确实发生了结构相变，是从常压正交相转变为高压单斜相。我们通过对XRD精修给出了其状态方程随压力的变化及体弹模量。同时我们发现LiCuVO_4具有Jahn-Teller效应，由其Cu离子在CuO6八面体协同作用引起的。但是通过压力的作用，扭曲的CuO6八面体趋向于正八面体，因此我们认为，压力的作用可以降低Jahn-Teller效应作用。其次，我们对研究最广泛及最具代表性LiNiVO_4进行了原位Raman光谱方面的研究，发现在20GPa左右拉曼峰位出现了畸变，可能存在结构相变。随后对样品进行了同步辐射XRD的研究，证实了Raman光谱方面对结构相变的信息。利用XRD精修我们预测该结构相变是从常压的立方相由于高压的作用转变到了高压正交相。另一个被广泛关注的尖晶石结构的正极材料是LiMnVO_4。通过对其进行原位高压Raman光谱的实验和同步辐射实验，发现其在高压下也发生了结构相变，其相变序列为正交Na_2CrO_4型结构Phase-Ⅰ→立方尖晶石结构Phase-Ⅱ→Phase-Ⅲ→Phase-Ⅳ。这三种材料中，前两种发生的相变都是可逆的，只有LiMnVO_4卸压后得到了一个高压相结构。
In modern times, solution of the energy shortage problem need to been workedout in hurry. Because of that, the development of lithium-ion batteries have also gotwidely attention. In the lithium ion cathode performance comparison, the negativeselection of carbon material technical standard both in theory and practicalapplications are already very mature, and the cathode material choice also needgreatly improvement. Recently, GT-K.Fey et al first synthesized by inverse spinelstructure of LiNiVO_4, the Li+intercalation and deintercalation process can reach4.8V,create a5V lithium ion battery cathode material of precedent. Since then has a spinelstructure of a class of cathode materials for lithium ion batteries into the scientificresearcher of vision. This paper selects three representative hotspot poly anion lithiumion battery cathode material LiMVO_4(M=Cu, Ni, Mn). The ternary cuprate oxidematerial having an inverse spinel structure, but each has different structure symmetry.Firstly, a widely reported material LiCuVO_4。It is not only just5V cathode material,but also due to its orthorhombic inverse spinel structure in Cu-O-Cu special bondingproperties as well as the unit cell structure information, which has been the attentionof magnetism. We also selected the LiCuVO_4at ambient with orthorhombic inversespinel structure of the sample, and carries out the in situ high pressure Ramanspectroscopy experiment, found in the20GPa Raman peak partially disappeared, andwith the emergence of new peak. And the shift of peak position are also varyingdegrees of distortion. We can conclude that the occurrence of the structure phasetransition. Synchrotron radiation XRD research shows that20GPa occur structuralphase transition, is from the atmospheric orthorhombic phase transition forhigh-pressure monoclinic phase. At the same time we discovered that the LiCuVO_4has Jahn-Teller effect, the Cu ion in the CuO6octahedron synergistic effects inducedby. But by the increasing of pressure, distortion of the CuO6octahedron incline to normal octahedron, so we think, pressure can reduce the Jahn-Teller effect. Secondly,we study the most extensive and most representative LiNiVO_4by in situ Ramanspectroscopy studies, found in the position of20GPa Raman peak appeared distortion,there may be a structural phase transition. Then the samples were studied bysynchrotron radiation XRD, confirmed that the Raman spectrum of structural phasetransition of information. The use of XRD pattern we predict the structure phasetransition is from the ambient cubic phase transform to the high-pressureorthorhombic phase. Another spinel type Cathode material which has been paid closeattention is LiMnVO_4. On the basis of the in situ high pressure Raman spectroscopyexperiments and synchrotron radiation experiments, found in the high pressure alsooccurred under the structural phase transition, through the XRD refinement, we getthe rule of phase transition: orthorhombic Na_2CrO_4tpye Phase-Ⅰ→Cubic spinel tpyePhase-Ⅱ→Phase-Ⅲ→Phase-Ⅳ. Among these three materials, the first two hasperformed a reversible phase transition, only LiMnVO_4can get a high pressure phasefrom decompression.
In modern times, solution of the energy shortage problem need to been workedout in hurry. Because of that, the development of lithium-ion batteries have also gotwidely attention. In the lithium ion cathode performance comparison, the negativeselection of carbon material technical standard both in theory and practicalapplications are already very mature, and the cathode material choice also needgreatly improvement. Recently, GT-K.Fey et al first synthesized by inverse spinelstructure of LiNiVO_4, the Li+intercalation and deintercalation process can reach4.8V,create a5V lithium ion battery cathode material of precedent. Since then has a spinelstructure of a class of cathode materials for lithium ion batteries into the scientificresearcher of vision. This paper selects three representative hotspot poly anion lithiumion battery cathode material LiMVO_4(M=Cu, Ni, Mn). The ternary cuprate oxidematerial having an inverse spinel structure, but each has different structure symmetry.Firstly, a widely reported material LiCuVO_4。It is not only just5V cathode material,but also due to its orthorhombic inverse spinel structure in Cu-O-Cu special bondingproperties as well as the unit cell structure information, which has been the attentionof magnetism. We also selected the LiCuVO_4at ambient with orthorhombic inversespinel structure of the sample, and carries out the in situ high pressure Ramanspectroscopy experiment, found in the20GPa Raman peak partially disappeared, andwith the emergence of new peak. And the shift of peak position are also varyingdegrees of distortion. We can conclude that the occurrence of the structure phasetransition. Synchrotron radiation XRD research shows that20GPa occur structuralphase transition, is from the atmospheric orthorhombic phase transition forhigh-pressure monoclinic phase. At the same time we discovered that the LiCuVO_4has Jahn-Teller effect, the Cu ion in the CuO6octahedron synergistic effects inducedby. But by the increasing of pressure, distortion of the CuO6octahedron incline to normal octahedron, so we think, pressure can reduce the Jahn-Teller effect. Secondly,we study the most extensive and most representative LiNiVO_4by in situ Ramanspectroscopy studies, found in the position of20GPa Raman peak appeared distortion,there may be a structural phase transition. Then the samples were studied bysynchrotron radiation XRD, confirmed that the Raman spectrum of structural phasetransition of information. The use of XRD pattern we predict the structure phasetransition is from the ambient cubic phase transform to the high-pressureorthorhombic phase. Another spinel type Cathode material which has been paid closeattention is LiMnVO_4. On the basis of the in situ high pressure Raman spectroscopyexperiments and synchrotron radiation experiments, found in the high pressure alsooccurred under the structural phase transition, through the XRD refinement, we getthe rule of phase transition: orthorhombic Na_2CrO_4tpye Phase-Ⅰ→Cubic spinel tpyePhase-Ⅱ→Phase-Ⅲ→Phase-Ⅳ. Among these three materials, the first two hasperformed a reversible phase transition, only LiMnVO_4can get a high pressure phasefrom decompression.
引文
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