鋁集流體腐蝕抑制劑和氧化還原穿梭添加劑用於鋰金屬電池中的死鋰再生

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研究生：	Teshager Mekonnen Tekaligne Teshager Mekonnen Tekaligne
論文名稱：	鋁集流體腐蝕抑制劑和氧化還原穿梭添加劑用於鋰金屬電池中的死鋰再生 An Aluminum current collector corrosion inhibitors and redox shuttle additive for dead lithium rejuvenating in lithium metal batteries
指導教授：	黃炳照 Bing-Joe Hwang 蘇威年 Wei-Nein Su
口試委員:	黃炳照 Bing-Joe Hwang 吳溪煌 She-Huang Wu 蘇威年 Wei-Nein Su 劉如熹 Ru-Shi Liu 張仍奎 Jeng-Kuei Chang 王迪彥 Di-Yan Wang
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：	英文
論文頁數：	266
中文關鍵詞：	水基電解液、5-甲酰基-8-羥基喹啉、酞菁、集電體、抑制效率、氧化還原添加劑、有機基電解液
外文關鍵詞：	Aqueous based electrolyte, 5-formyl-8-hydroxyquinoline, Current collector, Inhibition efficiency, Redox-Shuttle additive
相關次數：	點閱：206 下載：0
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摘要
採用非易燃的水基電解質的水性電池的發展具有降低能量儲存成本和提高安全性的潛力，使得這些電池可以在廣泛的應用中使用。鋁箔由於其高電導率、低成本、強大的電化學性能和低密度而經常被用作電池的陰極電流收集器。然而，隨著下一代電池的開發，嚴重的腐蝕對鋁電流收集器提出了新的挑戰，尤其是在迄今沒有有效添加劑的水性電解質中。於第一項工作中，我們成功地設計和合成了5-甲醛基-8-羥基喹啉（FHQ）作為鋁箔的有效防腐蝕劑。在含有FHQ添加劑的21m LiTFSI水性電解質中測量的每年毫米腐蝕速率（mmpy）為1.37×10-3 mmpy，比未修改的電解質的2.29×10-2 mmpy低得多。含有FHQ添加劑的Zn // LVPF電池提供了更高的容量保持率和平均庫倫效率。有趣的是，開發的添加劑在基於有機電解質的電池中也被證明可以有效防止鋁腐蝕。在第二項工作中，有趣的是，含有Pc添加劑的水電解液中的腐蝕電流密度（0.013微安）比不含Pc的腐蝕電流密度（0.302微安）低23倍。此外，Zn/LVPF電池被用來評估在水電解質中對其電池性能的腐蝕影響。在0.2℃的速率下，添加了Pc添加劑的Zn||LVPF電池在100次和200次循環後分別表現出較高的容量保持率和50.12%。不加Pc的電池顯示出更差的循環壽命，在40次循環後只有27.57%的容量保持率。此外，Pc可以防止有機電解質電池中的鋁腐蝕。 Pc添加劑可以通過雙重安全鈍化機制防止鋁腐蝕，包括其在鋁表面的物理吸附和電化學形成的AlPc-F鈍化層以及來自雙（三氟甲磺酰）亞胺陰離子的氟化物。
此外，鋰金屬電池中經常出現的性能劣化大多是由於無活性鋰（稱為死鋰）所致，它可以在固體電解質互溶形式和電隔離的金屬鋰中找到。迫切需要一種復甦機制來恢復死鋰以穩定鋰金屬電池效能。先前雖有已經識別出的氧化還原穿梭子因不穩定，導致過充保護時間短，或是氧化還原電位限制了它們在高電位正極材料（如NMC和LVPF）的電池中的使用。於最後一項工作，我們成功開發了一種新合成的化合物1,4-雙((三氟甲氧基)甲氧基)-2,5-二叔丁基苯（TFMB），並發現它具有穩定的氧化還原穩定媒介，其氧化還原電位為4.39V，能夠為鋰金屬電池提供過充保護，表明它有足夠的還原一致性。TFMB具有雙重穩定機制，能夠生成穩定、不溶性、堅固的LiF 固態電解質介面，以及恢復來自Cu/Li陽極的死鋰。在負極，氧化的TFMB（o-TFMB）將無活性的鋰（死鋰）轉化為活性的鋰，並將自己還原為還TFMB（r-TFMB），在充電時會在正極重新氧化為o-TFMB；去鋰化的陰極可由復甦的鋰離子重新鋰化，並在再生TFMB+。通過這種設計，使Cu箔陽極和NMC陰極所組成的無陽極電池展示了出色的循環壽命，進行86個循環後，具有高達99.01％的高庫倫效率和62％的容量保留率。然而，沒有添加劑的電解質容量保留率明顯較低，僅為6.58％，30個循環後的庫倫效率為89.73％。此外，在使用TFMB添加劑的Li//NMC電池中，以0.2 C速率進行循環充放電進行230圈後，高容量保留率為72.84％，平均庫倫效率為99.78%。然而，沒有添加劑的電解質容量保留率明顯較低，僅為3.92％，230個循環後的庫倫效率為96.34％。

Abstract
Developing aqueous batteries employing non-flammable water-based electrolytes can lower energy storage costs and improve security, allowing for using these batteries in various applications. Due to its excellent electrical conductivity, low cost, reliable electrochemical characteristics, and low density, aluminum foil is commonly used as a battery cathodic current collector.
However, severe corrosion raises significant problems for aluminum current collectors when next-generation batteries are developed, particularly given the lack of an efficient additive in an aqueous electrolyte. Furthermore, the performance deterioration frequently seen in lithium metal batteries is mainly caused by inactive lithium (more popularly referred to as dead lithium), which can be found in SEI forms and electrically segregated metallic lithium. A fundamental mechanism of retrieving dead lithium is urgently required to stabilize lithium metal batteries. The majority of redox shuttles that have been previously identified have either been unstable as redox shuttles, yielding in a short time of overcharge protection or had redox potentials that restricted their use to cells with higher potential positive electrode materials, such as NMC and LVPF.
In the first work, we successfully developed 5-formyl-8-hydroxyquinoline (FHQ), a potent corrosion inhibitor for aluminum foil.1 The corrosion inhibitor for aluminum foil, FHQ, has been devised and created. In the aqueous electrolyte of 21 m LiTFSI with the FHQ additive, the corrosion rate was measured in millimeters per year (mmpy), and it was substantially lower at 1.37 10-3 mmpy than it was at 2.29 10-2 mmpy in the unaltered electrolyte. The average Coulombic efficiency and capacity retention of the Zn/LVPF cell in the aqueous electrolyte with the FHQ additive is mis greater. Interestingly, an organic electrolyte also attests to the developed additive’s effectiveness at preventing Al corrosion.
In the second work, Interestingly, the corrosion current density (0.013 µA) in the aqueous electrolyte with Pc additive is 23 times less than that (0.302 µA) without Pc. Furthermore, Zn/LVPF cell was used to assess the corrosion impact on its battery performance in an aqueous electrolyte. Zn||LVPF cells at 0.2 C rate with Pc additive demonstrated higher capacity retention of 75% and 50.12% after 100 and 200 cycles, respectively. The battery without Pc showed a substantially worse cycle life with only 27.57% capacity retention after 40 cycles. Furthermore, Pc prevents aluminum corrosion in an organic electrolyte-based battery. Pc additive can prevent aluminum from corrosion by a dual-secure passivation mechanism, including its physical adsorption on the Al surfaces and electrochemically-formed AlPc-F passivation layer and fluoride from the bis(trifluoromethane sulfonyl)imide anion.
In the final work, we developed that the newly synthesized 1,4-bis((trifluoromethoxy)methoxy)-2,5-di-tert-butylbenzene (TFMB) is shown to be a stable redox shuttle with a 4.39V redox potential and provides overcharge protection in Li-metal batteries, suggesting good reductive consistency. The TFMB has a dual-secure mechanism enables it to generate stable and insoluble robust LiF SEI and revive the dead Li from the Cu/Li anode. At the negative electrode, the oxidized-TFMB (o-TFMB) converts inactive Li (dead Li) into active Li and itself to reduced-TFMB (r-TFMB) that will be re-oxidized to o-TFMB at the positive electrode during charging. The oxidation of dead Li by reverting to its original lithiation condition, regenerating the delithiated cathode TFMB+ at the cathode, and rejuvenating Li ion from inactive Li. Through this design, an anode-free battery using a Cu foil anode and NMC as a cathode displays an admirable lifespan of 86 cycles with a high Coulombic efficiency of 99.01% and capacity retention of 62%. However, the electrolyte without additives had much lower capacity retention, with only 6.58 % and an ACE of 89.73% after 30 cycles. Furthermore, after 230 cycles and 0.2 C-rate, the charge-discharge curve of a Li//NMC cell with TFMB additives exhibits high-capacity retention of 72.84% with an ACE of 99.78%. However, the electrolyte without additives had much lower capacity retention, with only 3.92% and an ACE of 96.34% after 230 cycles.

Table of Contents
摘要    i
Abstract    iii
Acknowledgment    vi
List of Figures    xii
Index of Tables    xvii
Index of Schemes    xviii
Index of Units and Abbreviations    xix
Chapter 1 General Background    1
1    Background of the study    1
2    Sources of Energy and Storage Devices    3
3    Aqueous and non-aqueous Rechargeable batteries    5
4    Current collector    9
5    Corrosion of current collector    10
6    Dead Lithium in Lithium metal batteries    12
Chapter 2 challenges, their mitigation, and reviving dead lithium for rechargeable batteries    15
1    Current collectors for rechargeable batteries    15
2    The main requirements of current collectors in lithium-ion batteries    16
3    Challenges and mitigation of current collector for rechargeable batteries    17
3.1    Current collector    17
3.2    Challenges of the current collector    21
3.3    Mitigation for deterioration of current collector    28
4    Challenges and Mitigation of Dead Li for LMBs    35
4.1    Challenges of high-performance LMBs    36
4.2    Mitigation of dead Lithium    41
5    Developing a corrosion inhibitor and redox shuttle additives    45
6    Dead lithium regeneration with redox shuttle additives for lithium metal batteries    49
7    Motivation and objectives of the study    52
7.1    The Motivation of the Study    52
7.2    Objectives of the Study    55
Chapter 3 Materials, experimental procedures, and characterization methodologies    57
1    Chemicals and Reagents    57
1    Cathode Material Preparation    58
2    Anode Current Collector Preparation    59
3    Synthesis of 5-formyl-8-hydroxyquinoline (FHQ)    59
5    Synthesis of 1, 1,4-bis((trifluoromethoxy)methoxy)-2,5-di-tert-butylbenzene (TFMB)    60
6    Electrolyte Preparation    61
7    Physicochemical Properties    62
8    Electrochemical Measurements    62
9    Morphological Evolution of in situ Deposited Li    63
10    SEI Components Characterization    64
Chapter 4 Inhibition of Aluminum Current Collector Corrosion in an Aqueous-based Battery by 5-Formyl-8-Hydroxyquinoline    65
1    Introduction    65
2    Results and Discussion    67
2.1    Properties assessment by computational analysis    67
2.2    The synthetic route    71
3    Electrochemical measurements    72
3.1    Measurements of Potentiodynamic    72
3.2    Measurement employing electrochemical impedance spectroscopy (EIS)    79
4    Surface analysis of aluminum    82
4.1    Surface characterization following chemical and electrochemical tests    82
4.2    Assessment of surface texture, size, and roughness    87
4.3    Composition analysis of the Al current collector surface    90
4.4    Al Surface current collector characterizations    94
5    Electrochemical Performance Test    97
6    Summary    106
Chapter 5 Designing a novel anticorrosion Phthalocyanine additive with a dual-secure prevention mechanism for an aluminum current collector in an aqueous-based battery    109
1    Introduction    109
2    Results and Discussion    112
2.1    Properties assessment by computational analysis    112
2.3    Electrochemical measurements and aluminum surface analyses    115
2.4    Electrochemical Performance Test    135
2.5    Mechanistic insight into corrosion prevention    140
3    Summary    146
Chapter 6 1,4-bis((trifluoromethoxy)methoxy)-2,5-di-tert-butylbenzene for lithium metal batteries as a novel Redox Shuttle additive for dead Li regeneration and overcharge protection    149
1    Introduction    149
2    Results and Discussion    152
2.1    Properties assessment by computational analysis    152
2.2    The synthetic route    153
2.3    Spectroscopic Characterization    154
2.4    Quantification of inactive Lithium    159
2.5    Electrochemical measurements    172
2.6    Overcharge Protection Performance    174
2.7    Cell Performance test    177
2.8    Surface analysis    181
2.9    Evaluation of Cu current collector's surface chemical composition after plating    184
3    Summary    186
Chapter 7: Conclusions and Perspectives    188
1    Conclusions    188
2    Perspective    190
References    194
List of Publications    235

                                

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全文公開日期 2028/07/11 (校內網路)
全文公開日期 2028/07/11 (校外網路)
全文公開日期 2028/07/11 (國家圖書館：臺灣博碩士論文系統)

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