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研究生： 吳哲亞
Wu, Che-Ya
論文名稱： 利用表面改質及摻雜技術應用於提升鋰離子電池材料循環穩定性及快速充放電能力
Surface Modification and Doping Techniques Applied in Lithium-ion Battery to Improve Cycle Stability and High-rate Capability
指導教授： 杜正恭
Duh, Jenq-Gong
口試委員: 黃炳照
Hwang, Bing-Joe
呂福興
Lu, Fu-Hsing
林姿瑩
Lin, Tzu-Ying
葉哲寧
Yeh, Che-Ning
蕭立殷
Hsiao, Li-Yin
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： 2024
畢業學年度： 112
語文別： 英文
論文頁數： 227
中文關鍵詞： 鋰離子電池 、正極材料 、負極材料 、表面改質
外文關鍵詞： Lithium-ion Battery, Cathode Material, Anode Material, Surface Modification
相關次數： 點閱：2  下載：0 
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    • 隨著人們對於能源的需求提升及環保意識的抬頭，儲能成為重要的課題，而在儲能的各種方法中，鋰離子電池展現高能量密度及高循環壽命的特性，被廣泛應用在電動車及儲能系統中。然而，為了使電池壽命進一步提升，參雜及表面改質等技術必須使用於鋰離子電池材料的改質中，在本論文中，透過不同的製程方法來提供提升鋰離子電池材料之性能。
    在正極材料方面，本研究提出硼摻雜鎳鈷錳三元氧化物層狀材料，透過共沉澱法進行材料的合成，再透過硼酸的添加，來進行硼參雜，研究發現硼參雜會影響(003)的面間距，進而透過充放電的結構穩定性來提升電化學穩定性，另外在參雜後的粉末還提升快速充放電能力，可得知藉由硼元素進行參雜能有效的改善鎳鈷錳層狀氧化物的性能。
    在負極方面可分成兩部分，包含高能量密度之合金型材料開發及快充鈦基材料開發，在合金型材料開發中，本研究提出形貌控制、表面碳批覆及結構設計等手法來緩解合金型材料充放電時所遇到的體積膨脹之問題，可以得到更高循環壽命之材料，而在經過碳複合材料添加後，材料快速充放電的能力也能進一步大幅提升。快充鈦基材料開發中，更進一步導入大氣電漿表面處理技術，透過大氣電漿對電極進行直接處理，探討電極內導電碳、黏結劑及活性物的改變。結果發現大氣電漿可以使導電碳進行氮元素摻雜、黏結劑官能基修飾及活性物氧空缺製造，透過這些手法的改質材料皆能提升鋰離子電池材料之充放電穩定性及快速充放電能力。
    在本論文中提出多種有效之材料改質手法應用在鋰離子電池材料中，在鋰離子電池材料製備中，元素摻雜及表面改質技術能大幅度提升鋰離子電池的穩定性。總而言之，本論文嘗試多種不同的合成及改質技術，包含水熱法、共沉澱法、氣相沉積聚合、冷凍乾燥與大氣電漿等，來提升鋰離子電池正負極材料的穩定性及快充能力。

    In recent years, energy storage becomes a vital issue due to the demand of energy increasing and the awareness of carbon emissions reduction. Among all the energy storage system, lithium-ion batteries demonstrate high specific capacity and cycle stability. Consequently, lithium-ion batteries are applied in the field of electric vehicles and energy storage station. Nonetheless, doping and surface modification technologies should be applied in the materials treatment to further improve the cycle life and rate capability of the cell. In this thesis, various of fabrication methods are promoted to improve the electrochemical performance of lithium-ion batteries.
    In cathode materials, boron-doped NMC811 layer-type cathode material is proposed. NMC811 is fabricated by co-precipitate method, and boric acid is added as the precursor of boron. It is found that the adding of boron element influences the (003) d spacing, and the structure stability during charging and discharging, enhancing the cycle stability. Moreover, the changing of the d spacing also improve the high-rate capability of the NMC811 materials. It is confirmed that the NMC811 materials can be better improved via boron-doping technique.
    Studies on anode materials part can be divided into two parts, including alloy-type materials with high capacity and Ti-based with fast charging capability materials. In the development of alloy-type materials, morphology control, surface carbon coating, and structure design are promoted to resolve the volume expansion during charging and discharging. It is found that these strategies effectively improve the cycle stability of the materials. Moreover, the carbon composite design also enhances the high-rate capability of the alloy-type materials. On the other hand, Ti-based materials is modified through the treatment of atmospheric pressure plasma jet. In this study, electrode is directly treated with the plasma jet, and the changing of active materials, conductive carbon, and binder is characterized. The results demonstrate that the treatment of atmospheric pressure plasma jet induce N-doped carbon, oxygen vacancy in TiNb2O7 material, and functionalized PVDF binder. All these variations improve the performance of the cell, including cycle stability and high-rate capability.
    In this thesis, various strategies are proposed to be applied to the improvement of lithium-ion batteries materials. In the fabrication process of materials in lithium-ion batteries, element doping, and surface modification play the most important roles to improve the stability and high-rate capability of the lithium-ion batteries. In this thesis, various techniques via hydrothermal method, co-precipitate method, vapor deposition polymerization, freeze-drying process, and atmospheric pressure plasma jet techniques are adopted to enhance the electrochemical performance of lithium-ion batteries.

    Contents X List of Figures XIV List of Tables XXV Chapter1 Introduction 1 1.1 Background and History Lithium-ion batteries 1 1.2 Components in Li-ion batteries 2 1.3 Introduction of Cathode materials in Li-ion batteries 3 1.4 Introduction of Anode materials in Li-ion batteries 5 1.5 Motivation and Objective in this study 7 Chapter2 Literature Review 16 2.1 Reaction mechanisms in Lithium-ion batteries 16 2.1.1 Reaction mechanisms 16 2.1.2 Solid electrolyte interface 16 2.1.3 Energy density of the batteries 17 2.2 Introduction of NMC811 cathode material 18 2.2.1 The reaction mechanism of NMC811 cathode material 18 2.2.2 Critical Issues of NMC811 cathode material 19 2.2.3 Strategies to improve the NMC811 electrochemical performance 21 2.3 Introduction of Sn and Si-based anode materials 24 2.3.1 The reaction mechanism of Sn and Si-based anode material 24 2.3.2 Critical Issues Sn and Si-based anode material 26 2.3.3 Strategies to improve the Sn and Si-based anode electrochemical performance 29 2.4 Introduction of TiNb2O7 anode materials 33 2.4.1 The reaction mechanism of TiNb2O7 anode material 33 2.4.2 Critical Issues TiNb2O7 anode material 34 2.4.3 Strategies to improve the TiNb2O7 anode electrochemical performance 34 2.5 Overview of modification in development of Li-ion batteries materials in Duh’s Lab 36 2.5.1 Composite design 37 2.5.2 Morphology control 37 2.5.3 Dopants addition 38 2.5.4 Surface modification - Protective layer coating 38 2.5.5 Surface modification - Plasma treatment 39 Chapter3 Experiment Procedure 71 3.1 Materials preparation of NMC811 cathode 71 3.1.1 NMC811 precursor 71 3.1.2 NMC811 preparation – co-precipitate method 71 3.1.3 Preparation of NMC811 electrode 72 3.2 Materials preparation of SnS/N-doped carbon anode 73 3.2.1 SnS/N-doped carbon precursor 73 3.2.2 SnS/N-doped carbon preparation – hydrothermal method 73 3.2.3 Preparation of SnS/N-doped carbon electrode 74 3.3 Materials preparation of Si/N-doped carbon core-shell anode 75 3.3.1 Si/N-doped carbon precursor 75 3.1.2 Si/N-doped carbon preparation – vapor deposition polymerization method 75 3.3.2 Preparation of Si/N-doped carbon electrode 76 3.4 Materials preparation of Si/ Cellulose nanofiber 3D-net anode 76 3.4.1 Preparation of cellulose nanofiber solution from waste rice straw 76 3.4.2 Si/ Cellulose nanofiber preparation – freeze-drying method 77 3.4.3 Preparation of Si/ Cellulose nanofiber electrode 78 3.5 Materials preparation of TiNb2O7 anode materials 78 3.5.1 TiNb2O7 precursor 78 3.5.2 TiNb2O7 preparation – solid-state method 78 3.5.3 Preparation of TiNb2O7 electrode 79 3.5.4 Atmospheric pressure plasma jet treatment on the electrode 79 3.6 Coin cell Assembly 80 3.6.1 NMC811 80 3.6.2 SnS/N-doped carbon 81 3.6.3 Si/N-doped carbon 81 3.6.4 Si/ Cellulose nanofiber 81 3.6.5 TiNb2O7 82 3.7 Electrochemical analysis 82 3.7.1 Cycle and C-rate test 82 3.7.2 Cyclic Voltammetry (CV) test 82 3.7.3 Electrical impedance measurements (EIS) test 82 3.8 Materials characterization and analysis 83 3.8.1 X-ray Diffractometer (XRD) 83 3.8.2 Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) 83 3.8.3 Thermo gravimetric analysis (TGA), Differential scanning calorimetry (DSC) 83 3.8.4 Fourier Transform Infrared Spectrometer (FT-IR) 83 3.8.5 Raman 84 3.8.6 High-resolution X-ray photoelectron spectroscopy (HR-XPS) 84 3.8.7 Scanning Electron Microscope (SEM) 84 3.8.8 Transmission Electron Microscopy (TEM) 84 3.8.9 Contact angle 84 3.8.10 Brunauer-Emmett-Teller (BET) 85 3.8.11 Photoluminescence spectroscopy (PL) 85 3.8.12 Optical emission spectroscopy (OES) 85 Chapter4 Improving NMC811 Cathode Material via Boron doping and the Tuning (003) interplanar 91 4.1 Synthesis Reaction 91 4.2 B-doped NMC811 characterization 93 4.3 Electrochemical performance of B-doped NMC811 in Li-ion battery 95 4.4 Ex-situ analysis of B-doped NMC811 in Li-ion battery 97 4.5 Short Summary 99 Chapter5 Improving Alloy-type Cathode Material via Morphology Control, Surface Coating, and Structure Design 111 5.1 Synthesis reaction of SnS/N-doped carbon and materials characterization 111 5.2 Electrochemical performance of SnS/N-doped carbon in Li-ion and Na-ion battery 115 5.3 Synthesis reaction of Si/N-doped carbon and materials characterization 117 5.4 Electrochemical performance of Si/N-doped carbon in Li-ion 121 5.5 Si/nanocellulose characterization 124 5.6 Electrochemical performance of Si/nanocellulose in Li-ion 129 5.7 Post cycle analysis of the electrode 132 5.8 Short summary 134 Chapter6 Improving TiNb2O7 Anode Material via Atmospheric Pressure Plasma Treatment 156 6.1 Plasma Diagnosis 156 6.2 TiNb2O7, PVdF, and electrode characterization 157 6.3 Electrochemical performance of TiNb2O7 in Li-ion 167 6.4 Short summary 173 Chapter7 Conclusions 188 References 190 Publication list 226

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