鋰離子電池正極材料LiNi0.75-x-yMgyCo0.25MnxO2的相轉換、價數變化與電化學特性

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研究生：	廖珮芸 Pei-Yun Liao
論文名稱：	鋰離子電池正極材料LiNi0.75-x-yMgyCo0.25MnxO2的相轉換、價數變化與電化學特性 Phase Transition, Oxidation State and Electrochemical Characterization of LiNi0.75-x-yMgyCo0.25MnxO2 Cathode Materials for Li-ion Batteries
指導教授：	杜正恭 Jenq-Gong Duh
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2008
畢業學年度：	96
語文別：	英文
論文頁數：	159
中文關鍵詞：	鋰電池、結構變化、正極材料、吸收圖譜
外文關鍵詞：	Li-ion battery, structural transition, cathode, XAFS
相關次數：	點閱：4 下載：0
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LiNiO2 is one of the most attractive materials with the lower cost and higher discharge capacity to replace commercial LiCoO2 cathode material for Li-ion batteries. Nevertheless, due to the undesired capacity fading upon cycling and lower thermal and structural stability, transition metals, such as cobalt and manganese, are substituted for nickel to improve the properties LiNi0.75-xCo0.25MnxO2 materials. In this study, the structural changes for LiNi0.75-xCo0.25MnxO2 (x =0.1, 0.15 and 0.25) were investigated by synchrotron based in situ X-ray technique, along with the electrochemical measurements.
In situ XRD data of LiNi0.65Co0.25Mn0.1O2 upon charge showed that there were two hexagonal phases, H1 and H2, which could be recognized by tracking the changes of (003) peak. The lattice parameter “c” of new H2 phase was larger than that of original H1 phase, while the parameters “a” and “b” of H2 were smaller than those of H1. In fact, the phase boundary of H1 and H2 was smeared in LiNi0.6Co0.25Mn0.15O2 and LiNi0.5Co0.25Mn0.25O2, and a single-phase reaction was observed. The difference in phase transition was attributed to more degree of defects induced by the increase in Mn content. In addition, the changes of lattice parameters could be explained by the balance between ionic radius and the repulsive force of the layer-structured material.
The X-ray absorption near edge structure (XANES) indicated the initial valences in Li1-xNi0.5Co0.25Mn0.25O2 were +2/+3, +3 and +4 for Ni, Co, and Mn, respectively. The main redox reaction during delithiation was achieved by Ni (i.e. Ni2+□Ni3+ followed by Ni3+ □Ni4+). The oxidation states of Co and Mn remained Co3+ and Mn4+, respectively. The bond length of Ni-O decreased drastically, while the Co-O and Mn-O distances exhibited a slight change with the decrease of Li content in the electrode. It was further revealed all the second shell metal-metal (Ni-M, Co-M, and Mn-O) distances decreased due to the oxidation of metal ions.
For further improving the electrochemical performance and thermal stability, magnesium was chosen as dopant in Li[Ni0.6-yMgyCo0.25Mn0.15]O2 cathode materials. LiNi0.6-yMgyCo0.25Mn0.15O2 (y =0~0.08) were successfully synthesized via the mixing hydroxide method. These materials exhibited □-NaFeO2 structure as indicated by the XRD patterns. The intensity ratio of (003) to (104) showed that Mg substitution could reduce the cation mixing. The electrochemical performance, such as capacity retention, was also improved in both room temperature and 55 oC. The initial capacity of LiNi0.57Mg0.03Co0.25Mn0.15O2 was 214 mAh/g and had an excellent cyclic performance with only 7% capacity loss after 30 cycles. A combination of in situ synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) was used to study the phase transition and local environment change for LiNi0.57Mg0.03Co0.25Mn0.25O2 material charged to 5.2 V. In situ synchrotron X-ray diffraction patterns showed that the boundary of phase transition for H1 to H2 was more distinct in Mg-doped sample, indicating that the LiNi0.57Mg0.03Co0.25Mn0.15O2 material exhibited higher structural integrity. The improvements of both electrochemical retention and thermal stability were possibly attributed to the reduced cation mixing and complete structural changes. The high energy synchrotron XAS results showed that the main redox reaction during delithiation was achieved by Ni (i.e. Ni3+ □Ni4+), while the oxidation states of Co and Mn remained Co3+ and Mn4+ even charged to 5.2 V.

List of Tables...........................................................................................    III
Figures Caption......................................................................................    IV
Abstract...................................................................................................    XI
Chapter 1 Introduction..........................................................................    1
Chapter 2 Literature Review.................................................................    4
    2.1 Lithium Ion Batteries (LIB) and Cathode Materials ……..........    4
        2.1.1 Lithium Ion Batteries ........................................................    4
        2.1.2 Evolution in Lithium Ion Batteries...................................    5
        2.1.3 Charge-discharge Model in LIB........................................    7
        2.1.4 Cathode materials..............................................................    8
            2.1.4.1 The requirements of cathode materials....................    8
            2.1.4.2 Layer-structured LiCoO2 and LiNiO2......................    9
            2.1.4.3 Spinel LiMn2O4.......................................................    11
            2.1.4.4 Olivine LiFePO4......................................................    12
    2.2 Review on the Multi-cation LiMO2 (M = Transition metal)
Systems………………………………………………………...    14
        2.2.1 Evolution of LiNi1-x-yCoyMnxO2 materials........................    14
        2.2.2 Synthesis methods of LiNi1-x-yCoyMnxO2..........................    17
        2.2.3 Structure and phase of LiNi1-x-yCoyMnxO2........................    19
    2.3 Experimental techniques and related researches ........................    20
        2.3.1 Phase transition and in situ synchrotron X-ray diffraction
studies for cathode materials...........................................    20
        2.3.2 X-ray Absorption Spectroscopy........................................    23
Chapter 3 Experimental........................................................................    46
    3.1 Powder synthesis.........................................................................    46
    3.2 Characterization and analysis…………………………………..    49
        3.2.1 Thermal analysis...............................................................    49
        3.2.2 Compositional evaluation………………………………..    49
        3.2.3 Phase identification…………………………………..….    49
        3.2.4 Morphological observation and particle size distribution.    49
        3.2.5 Electrochemical characterization……….………..……....    50
        3.2.6 Thermal stability………………………………..………..    50
        3.3.7 In situ synchrotron X-ray diffraction…………….……....    51
        3.3.8 X-ray absorption spectroscopy…………….………….....    52
Chapter 4 Investigation on the Phase Transitions and Valence
Changes of LiNi0.75-xCo0.25MnxO2 Cathode Materials
during Cycling..........................................................................    58
    4.1 Introduction  ………………………………………………….    58
    4.2 Structural Changes of LiNi0.65Co0.25Mn0.1O2 Materials…...……    58
        4.2.1 Phase identification of the pristine LiNi0.65Co0.25Mn0.1O2.    58
        4.2.2 Electrochemical performance……………………….…..    59
        4.2.3 In situ XRD study of Li/LiNi0.65Co0.25Mn0.1O2 cell upon
charge…………………………………………………….    59
    4.3 In-situ Synchrotron X-ray Studies of LiNi0.6Co0.25Mn0.15O2
Cathode Materials during the 1st cycle …………………………    70
        4.3.1 Phase identification…………………………………...…    70
        4.3.2 In situ synchrotron XRD investigation upon charge…….    70
        4.3.3 Lattice constants ……………………………………..…    72
        4.3.4 In situ synchrotron XRD investigation upon discharge…    73
    4.4 Structural investigation of Li1-xNi0.5Co0.25Mn0.25O2 by in situ
XAS and XRD measurements …………………………….……    85
        4.4.1 Electrochemical performance……………………………    85
        4.4.2 K-edge XANES analysis of pristine
LiNi0.5Co0.25Mn0.25O2……………..................................…    85
        4.4.3 In situ XANES study ……………………………………    86
        4.4.4 In situ EXAFS…………………………………………...    87
        4.4.5 Phase change during charge…………………………..…    88
    4.5 The influence of Mn content on structural changes for
LiNi0.75-xCo0.25MnxO2 materials………................................……    105
Chapter 5 Investigation on the Effects of Mg-doped in
LiNi0.6-yMgyCo0.25Mn0.15O2 Cathode Materials......................     108
    5.1 Introduction ....…………………………………………….……    108
    5.2 Microstructure and Electrochemical performance of Mg-doped
LiNi0.6-yMgyCo0.25Mn0.15O2 (y = 0, 0.01, 0.03, 0.05 and 0.08)
cathode materials………………………………………………    109
    5.3 The improved structural and thermal properties of Mg-doped
LiNi0.6-yMgyCo0.25Mn0.15O2 cathode materials (y=0 and 0.03)…    116
        5.3.1 Phase identification……………………………………...    116
        5.3.2 Electrochemical performance…………………………....    116
        5.3.3 Structural stability and Phase transition ……………...…    117
        5.3.4 Thermal stability…………………………………………    119
    5.4 Investigation on the Valence Change and Local Structure at
over-charged state by In Situ XAFS for
LiNi0.57Mg0.03Co0.25Mn0.15O2 Material ……………………….…    130
        5.4.1 Valences of transition metals in the pristine
LiNi0.6Co0.25Mn0.15O2 and LiNi0.57Mg0.03Co0.25Mn0.15O2
Powders………………………………………………...…    130
        5.4.2 In situ XANES spectra………………………………...…    130
        5.4.3 Changes of oxidation states during charge………………    131
        5.4.4 I In situ EXAFS spectra……………………………….…    132
Chapter 6 Conclusions..........................................................................    144
References................................................................................................     148

                                

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