Li-Nafion黏著劑均勻包覆NCM正極材料之研究｜國立臺灣科技大學博碩士論文系統

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研究生：	林元凱 Yuan-Kai Lin
論文名稱：	Li-Nafion黏著劑均勻包覆NCM正極材料之研究 Research on Conformal Coating of Li-Nafion Binder on NCM Positive Electrode Materials
指導教授：	黃炳照 Bing-Joe Hwang
口試委員:	吳溪煌 She-Huang Wu 蘇威年 Wei-Nien Su 潘俊仁 Chun-Jern Pan 林明憲 Ming-Hsien Lin 黃炳照 Bing-Joe Hwang
學位類別：	博士 Doctor
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	中文
論文頁數：	146
中文關鍵詞：	高鎳正極材料、Li-Nafion 、高倍率充放性能、循環充放電穩定性
外文關鍵詞：	Ni-rich Positive Electrode Materials, Li-Nafion, Rate performance, Cycle Stability
相關次數：	點閱：167 下載：0
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全球主要經濟體積極推動降低對石化燃料的需求，促使新一波的能源轉型，而在發展轉型的路線上，提升鋰離子二次電池的能量密度成為重要的課題。高鎳正極材料具有超過210 mAh/g的高能量密度，因此而受到關注。但隨著鎳含量的提升，在充放電過程中，高鎳正極材料的劣化與容量的衰退也更為嚴重。黏著劑為鋰離子二次電池中不可或缺的元件，但目前商品化的PVDF僅提供物理性的黏合作用，未能對電極電化學性能有加成綜效。
在本研究中，選用具有陽離子傳導特性的Li-Nafion做為鋰離子二次電池高鎳正極材料 (NCM) 的粘著劑，並通過機械融合法將活性碳材均勻的包覆在 NCM表面 (NCM@C)，從而優化了Li-Nafion在NCM@C表面上的包覆均勻性，進而降低電極內的介面阻抗。經由電化學測試，在6C速率下，NCM@C可獲得153.1 mAh/g放電容量，遠優於NCM使用傳統混漿電極的134.3 mAh/g。均勻的包覆不僅提升了倍率放電的性能，也延緩了電解液與正極材料表面的反應，而有較好的循環放電表現。在1C充放電速率下測試100次循環後，NCM@C的容量保持率為91%，優於傳統混漿NCM電極的88 %，進一步將充放電速率提升至6C經過100次循環後，NCM@C的容量保持率與傳統混漿的NCM電極比較由74 %提升至85 %，在高倍率放電下，均勻塗層改善的效果更加顯著。我們發現透過正極材料的表面塗層，來改善電極內的介面阻抗，可以提高倍率放電性能和循環壽命。這個研究中所使用的表面改質方法，無須經過多餘的清洗或是熱處理，提供一種快速、且穩定的操作技術，簡化了處理的程序與降低成本。儘管在一般低速充放電的電池使用狀況下效果較不顯著，但在高倍率下的充放電性能與循環壽命提升極為顯著，這為需要快速充放電能力的應用提供了一個具有潛力的方向。
最後本研究也顯示了在室溫下，使用Li-Nafion同時做為黏著劑與高分子電解質的測試，做為未來高分子電解質應用的方向。

Major global economies are actively pushing for a reduction in the demand for fossil fuels, leading to a new era of energy transformation. In the course of developing this transition, enhancing the energy density of lithium-ion batteries has become a crucial challenge. Nickel-rich positive electrode materials have attracted attention due to their high energy density exceeding 210mAh/g. However, as the nickel content increases, the degradation and capacity decay of nickel-rich positive electrode materials become more severe during the charging and discharging process. Additionally, binders are indispensable components in lithium-ion secondary batteries. However, the currently commercialized PVDF (polyvinylidene fluoride) only provides physical adhesion, lacking other desirable properties.
In this study, a novel process was developed for the conformal coating of a lithium-ion conductive lithiated Nafion (Li-Nafion) binder on a nickel-rich positive electrode material, namely LiNi0.83Co0.12Mn0.05O2 (NCM), for lithium-ion batteries (LIBs). Specifically, mechanofusion was first performed to first fabricate an active carbon coating (Super-P) over the surface of NCM, named as NCM@C, thereby optimizing the Li-Nafion coating on NCM@C and reducing the interface impedance between Li-Nafion and NCM. The electrochemical test results revealed that the 6C discharge capacity of NCM@C increased from 134.3 mAh/g to 153.1 mAh/g following the mechanofusion treatment, verifying that conformal and uniform Li-Nafion coating improved discharge rate performance as well as mitigated interactions between the electrolyte and positive electrode materials surface, leading to better cycle discharge performance. After 100 cycles at 1C charge/discharge tests, NCM@C boosted its capacity retention from 88% to 91%. Furthermore, after conducting 100 cycles of testing at a charge-discharge rate of 6C, the capacity retention of NCM@C increased from 74% to 85%. The improvement in the uniform coating had an even more pronounced effect under high-rate discharge conditions. This study confirmed that a positive electrode materials coating with conformal and high uniformity enables the alleviation of interface impedance between Li-Nafion and NCM, thereby increasing the discharge rate performance and cycle life of batteries. The surface modification method utilized in this study offers a fast and stable operational technique without excessive washing or heat treatment, thereby reducing processing steps and costs. Although the effects may not be significant under typical low-rate charge-discharge conditions, there is a notable improvement in charge-discharge performance and cycle life under high-rate conditions. This provides a promising direction for applications requiring rapid charge and discharge capabilities.
In the final part of this study, the testing of Li-Nafion as both a binder and a polymer electrolyte at room temperature, serving as a reference for future applications of polymer electrolytes.

目錄
摘要    I
ABSTRACT    II
誌謝    IV
目錄    V
圖目錄    VIII
表目錄    XV
第 1 章    緒論    1
1.1    前言    1
1.2    鋰離子二次電池的應用    3
1.3    淨零碳排 (Net‐zero Emissions)    5
1.4    鋰離子二次電池工作原理概述    8
1.4.1    鋰離子二次電池負極材料 (Negative electrode materials)    10
1.4.2    鋰離子二次電池正極材料 (Positive electrode materials)    11
第 2 章    文獻回顧    13
2.1    金屬氧化物正極材料的演進    13
2.1.1    三元金屬氧化物正極材料的發現    14
2.1.2    鎳含量對鎳鈷錳三元正極材料的影響    17
2.1.3    高鎳正極材料的挑戰    20
2.1.3.1    陽離子錯位效應 (Cation Mixing)    23
2.1.3.2    高鎳正極材料的表面重建 (Surface reconstruction)機制    27
2.1.3.3    正極-電解液介面層 (Cathode electrolyte interphase CEI)    29
2.1.3.4    微裂紋結構 (Microcrack)    30
2.1.3.5    熱穩定性及安全性 (Thermal stability)    32
2.1.4    高鎳正極材料的表面修飾    34
2.2    鋰離子二次電池中的高分子黏著劑 (Binder)    37
2.3    機械融合法 (Mechanofusion)    41
2.4    研究動機    43
第 3 章    實驗方法及儀器    46
3.1    實驗藥品及化學品    46
3.2    實驗儀器及設備    46
3.3    實驗步驟    47
3.3.1    黏著劑Li-Nafion的製備    47
3.3.2    高鎳正極材料NCM表面修飾    48
3.3.3    NCM與NCM@C電極製備    48
3.4    電化學性能測試    50
3.4.1    鈕扣型電池組裝步驟    50
3.4.2    充放電測試條件    51
3.4.3    交流阻抗譜分析    51
3.5    材料鑑定與特性分析    53
3.5.1    傅立葉轉換紅外光譜儀 (FT-IR)    53
3.5.2    水滴接觸角分析    54
3.5.3    X-ray粉末繞射分析    55
3.5.4    場發射掃描式電子顯微鏡形貌與元素分析(SEM/EDS)    56
第 4 章    材料形貌與結構分析    58
4.1    Li-Nafion FT-IR結構分析    58
4.2    Li-Nafion做為NCM正極材料黏著劑的電極表面分析    59
4.3    經由Mechanofusion進行NCM表面修飾    61
4.4    Li-Nafion均勻性的差異與比較    65
第 5 章    Li-Nafion包覆層對正極材料的電化學性能影響    70
5.1    高速充放電循環比較    70
5.2    NCM與NCM@C以PVDF黏著劑之倍率性能比較    75
5.3    NCM與NCM@C以Li-Nafion黏著劑之倍率性能比較    81
5.4    NCM與NCM@C在不同充放電速率之循環壽命比較    86
5.5    在1C充放電速率循環過程之EIS分析    90
5.6    充放電循環前、後之電極XPS分析    96
5.7    以Li-Nafion做為黏著劑及隔離膜系統測試    100
第 6 章    結論    105
第 7 章    未來展望    107
第 8 章    參考文獻    109
第 9 章    附錄    119
附錄1.    119
附錄2.    122
附錄3.    123
附錄4.    124
附錄5.    127

圖目錄
Figure 1 1 2019~2030 market demand for Li-ion Battery by application10.    3
Figure 1 2 2000 and 2018 Li-ion Battery sales11.    4
Figure 1 3 Lithium-ion batteries placed on the global market (cell level, tonnes)13.    5
Figure 1 4 Key milestones in the pathway to net zero14.    7
Figure 1 5 Battery demand growth in transport and battery energy density in the NZE14.    8
Figure 1 6 A schematic illustration of LixC6/Li1−xCoO2 lithium-ion cell15.    9
Figure 1 7 Representative schematic of the main challenges associated with Li metal anode: (a) short circuit induced by Li dendrites, (b) formation of dead Li, and (c) development of thick and mechanically unstable SEI16.    11
Figure 2 1 Unit cell constants a, c and cell volume with the global phase diagram as a function of lithium concentration x in LiXCoO222.    13
Figure 2 2 Structure of layered lithium transition metal oxide materials with Ni/Li exchange26.    14
Figure 2 3 Schematic of d-electron levels of NCM materials28.    15
Figure 2 4 Compositional phase diagrams of lithium stoichiometric-layered transition-metal oxide: LiCoO2-LiNiO2-LiMnO231.    17
Figure 2 5 Comparison of the energy diagrams of LiCoO2, LiNiO2, and LiMnO232.    18
Figure 2 6 The relationship between discharge capacity and thermal stability and after 100 cycles capacity retention of difference NCM materials34, 35.    19
Figure 2 7 Illustrations of crystal structures relevant to the layered Ni-rich materials36.    21
Figure 2 8 Phase diagrams proposed from experimental and computational studies25.    22
Figure 2 9 Challenges of nickel-rich layered oxide positive electrode material.    22
Figure 2 10 Schematic of device for preparing transition metal hydroxides precursor by continuous co-precipitation40.    25
Figure 2 11 Effect of pH on the concentration of (Ni(NH3)n)2+, (Mn(NH3)n)2+, and (Co(NH3)n)2+ complexness41.    25
Figure 2 12 Schematic diagram of samples with different Li/TM ratios of 1.00 (E00), 1.06 (E06), and 1.12 (E12) indicating the Li/Ni mixing ratio, shrinkage, and enlargement of TMO6 and expansion and contraction of Li slab42.    27
Figure 2 13 Purpose mechanism of Oxygen Evolution Reaction (OER)43.    28
Figure 2 14 Schematic of surface change with the formation of residual lithium exposure in the Air47.    30
Figure 2 15 Schematic of CEI formation mechanism31.    30
Figure 2 16 Schematic of microcrack with difference nickel contain50.    32
Figure 2 17 Schematic diagram of the mechanism driving the cation transfer in two cases: (a) oxygen vacancies and (b) thermal expansion of the Li slab55.    33
Figure 2 18 (a) Synthesis scheme of organic CEI precursor for NCM811, (b) electrochemical performance of NCM811 with artificial sulfonate CEI, (c) XPS results for cycled electrodes.    36
Figure 2 19 Schematic illustration of the change in the network structure between day one slurry (left) and day seven slurry (right).    38
Figure 2 20 Structure of poly(vinylidenefluoride-hexafluoro propylene).    39
Figure 2 21 Structure of lithiated Nafion.    40
Figure 2 22 (a) Schematic diagram for the principle of cation exchange polymer coating on the LiMn2O4 electrode to capture dissolved Mn2+ ions. (b) Ion exchange reaction between H+ ions on the Nafion ionomer and Mn2+ ions.    40
Figure 2 23 The mechanofusion system.    42
Figure 2 24 SEM micrographs and EDS mapping of Al on NCA coated with 1% Al2O3 (A)、(a) and Al on NCA coated with 2% Al2O3 (B)、(b)84.    43
Figure 3 1 The flowchart of NCM and NCM@C electrode fabrication.    50
Figure 3 2 The composition of the coin cell.    51
Figure 3 3 Simplified equivalent circuit of a lithium-ion battery half-cell85.    52
Figure 3 4 Equivalent circuit of a lithium-ion battery85.    53
Figure 3 5 Michelson interferometer86.    54
Figure 3 6 Illustration of contact angles87.    55
Figure 3 7 Schematic representation of the Bragg’s scattering88.    56
Figure 3 8 Signals generated when a high-energy beam of electrons interacts with a sample89.    57
Figure 4 1 Titration curve of 0.1N LiOH with 60g H-Nafion.    58
Figure 4 2 FT-IR spectra of the Nafion film in difference forms.    59
Figure 4 3 (a) SEM images of NCM with Li-Nafion binder electrode and (b) is the larger magnification images, the corresponding EDS mappings of nickel (c), fluorine (d), cobalt (e), carbon (f).    60
Figure 4 4 Cross-sectional SEM/EDS analysis of pristine NCM with Li-Nafion binder electrode, red dot is the signal of Ni element and green dot is the signal of F element.    61
Figure 4 5 (a) SEM images of pristine NCM powder and (b) SEM images of the NCM powder with Super-P (NMC@C) after mechanofusion process.    62
Figure 4 6 The particle size distribution was analyzed by laser particle size analyzer.    63
Figure 4 7 Powder XRD profile of NCM and NCM@C.    64
Figure 4 8 Contact angle with water on different positive electrode materials. (a) Bare NCM and (b) NCM@C.    65
Figure 4 9 (a) SEM images of NCM@C with Li-Nafion binder electrode and (b) is the larger magnification images, the corresponding EDS mappings of nickel (c), fluorine  (d), cobalt (e), carbon (f).    66
Figure 4 10 Cross-sectional SEM/EDS analysis of NCM@C with Li-Nafion binder electrode, red dot is the signal of Ni element and green dot is the signal of F element.    67
Figure 4 11 SEM/EDS images of NCM and NCM@C electrodes after FIB treatment.    68
Figure 4 12 Schematic diagram of Li-Nafion coating with NCM and NCM@C powders.    68
Figure 4 13 Schematic diagram of tape peeling test (a), test results of NCM and NCM@C electrodes with Li-Nafion binder (b).    69
Figure 5 1 6C charge/discharge cycling test of NCM@C with Li-Nafion and PVDF as binder.    71
Figure 5 2 NCM@C with Li-Nafion and PVDF as binder at 6C rate after 100 cycles discharge curve.    71
Figure 5 3 The images of the battery disassembly after 100 cycles of testing at a 6C rate.    72
Figure 5 4 NCM@C with different binders SEM images of Li metal negative electrode after 6C charge-discharge cycles, where (a) (b) (c) represent Li-Nafion and (d) (e) (f) represent PVDF.    73
Figure 5 5 A schematic diagram illustrating the formation of SEI with (a) Li-Nafion and (b) PVDF.    74
Figure 5 6 C 1s XPS spectra and fitting results of NCM@C positive electrodes with Li-Nafion (a) and PVDF (b) binders after 100 cycles at the 6C charge/discharge.    75
Figure 5 7 Rate capability of (a) NCM and (b) NCM@C with PVDF binder.    76
Figure 5 8 NCM and NCM@C with PVDF binder discharge curve at 3C rate.    78
Figure 5 9 NCM and NCM@C with PVDF binder discharge curve at 6C rate.    78
Figure 5 10 6C charge/discharge cycling test of NCM and NCM@C with PVDF as binder.    80
Figure 5 11 NCM and NCM@C with PVDF binder at 6C rate discharge curve.    80
Figure 5 12 Rate capability of (a) NCM and (b) NCM@C with Li-Nafion binder.    82
Figure 5 13 NCM and NCM@C with Li-Nafion binder discharge curve at 3C rate.    84
Figure 5 14 NCM and NCM@C with Li-Nafion binder discharge curve at 6C rate.    85
Figure 5 15 Discharge capacity and columbic efficiency with cycle number at 1C charge/1C discharge. The filled marker with curve indicates 1C discharge capacity, and empty marker with curve indicates coulombic efficiency.    87
Figure 5 16 Discharge capacity and columbic efficiency with cycle number at 6C charge/6C discharge. The filled marker with curve indicates 6C discharge capacity, and empty marker with curve indicates coulombic efficiency.    88
Figure 5 17 The discharge curves of NCM and NCM@C at the 1st, 10th, and 100th cycle at 1C rate.    89
Figure 5 18 The discharge curves of NCM and NCM@C at the 1st, 10th, and 100th cycle at 6C rate.    90
Figure 5 19 Electrochemical impedance spectroscopy (EIS) plots of NCM@C and NCM with Li-Nafion binder after the first cycle (a), 10 cycles (b), and 100 cycles (c).    92
Figure 5 20 (a) The relationship between Z’ and square root of frequency (ω-1/2), (b) low-frequency region of NCM and (c) NCM@C with Li-Nafion binder.    95
Figure 5 21 XPS spectra of NCM and NCM@C electrodes with Li-Nafion binder before cycling test.    97
Figure 5 22 XPS spectra of NCM and NCM@C electrodes with Li-Nafion binder after 100 cycles at the 1C charge/discharge.    98
Figure 5 23 XPS spectra of the NCM and NCM@C electrodes with Li-Nafion binder after 100 cycles at 1C charge/discharges (a) Ni 2p (b) Co 2p (c) Mn 2p.    99
Figure 5 24 Picture of Li-Nafion separator.    100
Figure 5 25 Cycle test of Li-Nafion as binder and separator with NCM@C.    101
Figure 5 26 Charge and discharge curves of Li-Nafion as binder and separator with NCM@C.    102
Figure 5 27 37th cycle charge curve of Li-Nafion as binder and separator at 0.05C.    103
Figure 5 28 NCM@C electrode after 38 cycles with Li-Nafion binder and separator.    103
Figure 9 1 Electrochemical impedance spectroscopy (EIS) plots of NCM@C and NCM with PVDF binder after the first 6C charge/discharge.    119
Figure 9 2 (a) The relationship between Z’ and square root of frequency (ω-1/2), (b) low-frequency region of NCM and (c) NCM@C with PVDF binder.    120
Figure 9 3 NCM and NCM@C with Li-Nafion binder at C1s XPS after 6C cycling test.    122
Figure 9 4 The SEM images of NCM@C with Li-Nafion binder (a) (b), NCM with Li-Nafion binder (c) (d), NCM@C with PVDF binder (e) (f), and NCM with PVDF binder (g) (h).    123
Figure 9 5 After 100 cycles at 6C, the lithium metal anode of NCM@C with Li-Nafion binder SEM image (a), EDS mapping images Ni (b) C (c) O (d) F (e) P (f), and corresponding spectra (g).    124
Figure 9 6 After 100 cycles at 6C, the lithium metal anode of NCM@C with PVDF binder SEM image (a), EDS mapping images Ni (b) C (c) O (d) F (e) P (f), and corresponding spectra (g).    125
Figure 9 7 After 100 cycles at 6C, the lithium metal anode of NCM with Li-Nafion binder SEM image (a), EDS mapping images Ni (b) C (c) O (d) F (e) P (f), and corresponding spectra (g).    126
Figure 9 8 XPS spectra of NCM electrodes with Li-Nafion binder after 1C 200 cycles test.    127

表目錄
Table 1 1 Overview of the sequence of components for rechargeable lithium battery3.    2
Table 1 2 Characteristics of commercial Li-ion battery positive electrode materials19.    12
Table 2 1 Cation mixing of LiMnxNi1−xO2 prepared in difference atmosphere29.    16
Table 2 2 Cation mixing of difference LiNi0.8-xCoxMn0.2O2 prepared in air atmosphere30.    16
Table 2 3 Comparison of NCM surface modification methods and research motivation.    44
Table 5 1 Comparison of average voltage during 6C-rate discharge at the 1st, 10th, and 100th cycle using Li-Nafion and PVDF as binders with NCM@C.    72
Table 5 2 Comparison of rate capability between NCM and NCM@C with PVDF binder.    77
Table 5 3 Comparison of charging efficiency between NCM and NCM@C with PVDF binder at different rates.    79
Table 5 4 Comparison of average voltage during 6C-rate discharge at the 1st, 10th, and 100th cycle using PVDF as binders with NCM and NCM@C.    81
Table 5 5 Comparison of rate capability between NCM and NCM@C with Li-Nafion binder.    83
Table 5 6 Comparison of charging efficiency between NCM and NCM@C with Li-Nafion binder at different rates.    85
Table 5 7 Comparison of 1C rate discharge average voltage between NCM and NCM@C at 1st, 10th, 100th cycles.    89
Table 5 8 Comparison of 6C rate discharge average voltage between NCM and NCM@C at 1st, 10th, 100th cycles.    90
Table 5 9 EIS fitting results of the 1C charge/1C discharge tests on NCM and NCM@C with Li-Nafion as the binder following the 1st, 10th, and 100th cycles.    93
Table 5 10 NCM and NCM@C with Li-Nafion binder Li+ Diffusion coefficient calculation results and parameter conditions.    96
Table 5 11 Comparison of capacity and coulombic efficiency for different cycles.    104
Table 9 1 NCM and NCM@C with PVDF binder Li+ Diffusion coefficient calculation results and parameter conditions.    121


                                

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