電解質化學增強無陽極鋰金屬電池的電化學性能｜國立臺灣科技大學博碩士論文系統

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研究生：	Teklay T.M. Teklay Mezgebe Hagos
論文名稱：	電解質化學增強無陽極鋰金屬電池的電化學性能 Electrolyte Chemistry to Boost Electrochemical Performance of Anode-Free Lithium Metal Batteries
指導教授：	黃炳照 Bing-Joe Hwang 蘇威年 Wei-Nien Su
口試委員:	黃炳照 BING-JOE HWANG 蘇威年 WEI-NIEN SU 吳溪煌 SHE-HUANG WU 吳乃立 Nae-Lih Wu 鄧熙聖 Hsisheng Teng
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	203
中文關鍵詞：	無陽極鋰金屬電池、KPF6-TMSP 、電解質添加劑、鋰枝晶、電化學性能、不易燃的電解質、相位不穩定性、氧化穩定性、速率容量、低溫、黏度、離子電導率、羧酸酯溶劑
外文關鍵詞：	anode free lithium metal battery, KPF6-TMSP, electrolyte additives, lithium dendrite, electrochemical performance, nonflammable electrolyte, phase instability, oxidative stability, rate capability, low temperature, viscosity, ionic conductivity, carboxylate ester solvents
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與傳統的鋰金屬電池(LMB)和鋰離子電池(LIB)相比，無陽極鋰金屬電池（AFLMB）的能量密度高且生產相對容易，因此是一個具有前景的新儲能裝置。此外，AFLMB也可被用作評估方法，能夠在短時間內篩選出適合的功能電解質。
六氟磷酸鉀和三（三甲基甲矽烷基）亞磷酸酯被用作電解質添加劑，以增強基於Cu || NMC111電池構型的無陽極鋰金屬電池（AFLMB）的電化學性能。已經使用市售碳酸鹽電解質（1M LiPF6-EC / DEC（1∶1，以體積計））研究了雙添加劑的協同作用。在此，我們報導了具有2（按重量計）KPF6-2（按體積計）TMSP的雙重添加劑電解質可顯著改善Cu || NMC111電池配置的充放電容量、平均庫侖效率和保留容量。在第20個循環中，含有2種（按重量計）KPF6-2種（按體積計）TMSP添加劑的AFLMB電池保留了其初始容量的48％，而帶有市售電解質且不含添加劑的參考電池僅達到了14％。使用自製的電解質可提高性能，這歸因於KPF6的自癒靜電屏蔽（SHES）效果，可防止枝晶生長，使用TMSP進行沖洗並通過五氟化磷（PF5）的反應除去商用LiPF6碳酸鹽電解質產生的氫氟酸（HF）。這項研究為開發無陽極鋰金屬電池的功能性電解質添加劑提供了更廣闊的視野。
在我們的第二項工作中，溶解在氟化碳酸鹽（碳酸氟亞乙酯（FEC））和部分氟化醚（1,1,2,2-四氟乙基-2,2,3,3-四氟丙基醚（TTE））中的LiPF6已據報導，由於其較寬的電化學窗口與不可燃的特性以及穩定的富LiF固體電解質界面，在LMB的開發中是氟化電解質。但是，其相不穩定和高黏度限制了其實際應用。在這項工作中，開發了一種高級的碳酸甲乙酯（EMC）基氟化電解質（FEC / TTE / EMC中為1 M LiPF6（按體積計為3：5：2）），該電解質無相不穩定性並且具有更高的離子導電性、氧化穩定性和不燃性。與鋰金屬電池的無EMC電解液（Li || NCM111）相比，它具有更高的氧化電勢> 5.3 V，並且具有更高的倍率性能。同時，三元電解質還可在室溫下2.5-4.5 V的電位範圍內增強無陽極鋰金屬電池（AFLMB）的循環性能。在FEC / TTE / EMC（體積比為3：5：2）電解質中具有1 M LiPF6的Cu || NMC111電池可在充電和放電電流密度分別為 0.2和0.5 mA / cm2時，時的截止電壓中 4.5V，80個循環後提供40％的優異容量保持率和98.30％的平均庫侖效率（av. CE）。因此，我們使用無陽極的全電池配置（Cu || NMC111），開發了一種具有相穩定性的，堅固的，不可燃的，無相不穩定的電解質，該電解質具有較寬的氧化穩定性，較高的倍率能力和良好的循環性能。
在最終的工作中，充放電性能報告六氟磷酸鋰（LiPF6）在氟代碳酸亞乙酯（FEC），1,1,2,2-四氟乙基-2,2,3,3-四氟丙基醚（TTE）和碳酸乙基甲基酯（EMC）的混合物電解質用作開發鋰金屬電池的電解質。相對於商用電解質，它具有良好的鈍化能力、相穩定以及寬的電化學窗口，已被報導用作開發鋰金屬電池的電解質。相反地，由於其較低的離子電導率，高成本和高粘度阻礙了實際應用。因此，發展具有四元溶劑的電解質在EA / FEC / TTE / EMC中為1 M LiPF6（按體積計2：1：5：2），在MA / FEC / TTE / EMC中為1 M LiPF6（2：1：5: 2）分別通過加入乙酸乙酯（EA）和乙酸甲酯（MA）溶劑顯影：體積比為2：2）。值得注意的是，與FEC / TTE / EMC中的1 M LiPF6（按體積計3：5：2）和EC / DEC中1 M LiPF6的市售電解質（按體積計1：1）相比，電解質表現出較低的粘度和較高的離子電導率，擴大了AFLMB的使用溫度範圍。在0°C時，EA / FEC / TTE / EMC中的1 M LiPF6（以體積計為2：1：5：2）使用Cu‖NMC111經過40個循環後，電流密度為0.2 mA / cm2，可以保持電容的30％和平均庫侖效率95％（平均CE）。在室溫下的充電和放電電流密度分別為0.2和0.5 mA / cm2時，其截止電壓為4.5V，使用MA / FEC / TTE / EMC（體積比為2：1：5：2）中的1 M LiPF6電解質經過30個循環後的電池表現出58.50％的容量保持率和97.40％的平均庫侖效率。此外，EA / FEC / TTE / EMC中的1 M LiPF6（按體積計為2：1：5：2）在MCMB‖NMC111電池中具有出色的循環性能。

Anode free lithium metal battery (AFLMB) is an impressive and recent phenomenon in the era of energy storage devices due to their high energy density and relative ease of production compared to the traditional LMBs and LIBs. Also, AFLMB can be used as an evaluating method for screening out suitable functional electrolytes within a short time.
Potassium hexafluorophosphate and tris (trimethylsilyl) phosphite are applied as electrolyte additives to enhance the electrochemical performance of an AFLMB based on a Cu||NMC111 cell configuration. The synergistic effect of the dual additives has been investigated using a commercial carbonate electrolyte (1 M LiPF6-EC/DEC (1:1 by vol.)). Herein, we report that an electrolyte with the dual additive of 2 (by wt.) KPF6 - 2 (by vol.) TMSP significantly improves the charge/discharge capacity, average Coulombic efficiency (av. CE), and capacity retention of a Cu||NMC111 cell configuration. An AFLMB cell with 2 (by wt.) KPF6 - 2 (by vol.) TMSP additives retained 48% of their initial capacity at the 20th cycle, while the reference cell with the commercial electrolyte in the absence of additives reached only 14%. The enhanced performance using the prepared electrolyte is attributed to the self-healing electrostatic shielding (SHES) effect of KPF6 to prevent dendrite growth and the removal of hydrofluoric acid (HF) produced from the commercial LiPF6 carbonate electrolytes by the reaction of phosphorus pentafluoride (PF5) with water using TMSP. This study provides a broader vision in developing functional electrolyte additives for an anode-free lithium metal battery.
In our second work, the LiPF6 dissolved in fluorinated carbonate (fluoroethylene carbonate (FEC)) and partially fluorinated ether (1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether (TTE)) solvents has been reported to be a fluorinated electrolyte in the development of LMBs because of their wide electrochemical windows, nonflammable characteristics, and stable LiF-rich solid electrolyte interface. However, its phase instability and high viscosity limit its practical application. In this work, an advanced ethyl methyl carbonate (EMC)-based fluorinated electrolyte (1 M LiPF6 in FEC/TTE/EMC (3:5:2 by vol.)) is developed, which is free of phase instability and has higher ionic-conductivity, oxidative stability, and nonflammability. It has a higher oxidation potential > 5.3 V and better rate capabilities than the EMC-free electrolyte for lithium metal batteries (Li||NCM111). Meanwhile, the ternary electrolyte also enhances the cycling performance of anode-free lithium metal batteries (AFLMBs) within the potential range of 2.5-4.5 V at room temperature. The Cu||NMC111 cell with 1 M LiPF6 in FEC/TTE/EMC (3:5:2 by vol.) electrolyte delivers superior capacity retention of 40% and av. CE of 98.30% for 80 cycles with a cut-off voltage of 4.5 V at the charge and discharges current densities of 0.2 and 0.5 mA/cm2, respectively. Hence, we develop a robust nonflammable electrolyte free of phase instability having wider oxidative stability, high rate capability, and good cyclic performance using an anode-free full cell configuration (Cu||NMC111).

In the final work, the charge/discharge performance of an electrolyte consisting of lithium hexafluorophosphate (LiPF6) in a mixture of fluoroethylene carbonate (FEC), 1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether (TTE), and ethyl methyl carbonate (EMC) has been reported to be used as an electrolyte for the development of lithium metal batteries. It has a good passivating capability, phase stable, wide electrochemical windows relative to the commercial electrolyte. Conversely, its lower ionic conductivity, high cost, and high viscosity impeded from practical application. Hence, an electrolyte with the quaternary solvent of 1 M LiPF6 in EA/FEC/TTE/EMC (2:1:5:2 by vol.) and 1 M LiPF6 in MA/FEC/TTE/EMC (2:1:5:2 by vol.) is developed by adding ethyl acetate (EA) and methyl acetate (MA) solvent, respectively. Remarkably, thus electrolytes exhibit a lower viscosity and high ionic conductivity in comparison to 1 M LiPF6 in FEC/TTE/EMC (3:5:2 by vol.) and commercial electrolyte of 1 M LiPF6 in EC/DEC (1:1 by vol.) which extend the service-temperature range of AFLMB. At 0 °C, 1 M LiPF6 in EA/FEC/TTE/EMC (2:1:5:2 by vol.) provides capacity retention of 30 and 95% of the av. CE using the Cu||NMC111 after 40 cycles at a current density of 0.2 mA/cm2. The cell cycled with an electrolyte of 1 M LiPF6 in MA/FEC/TTE/EMC (2:1:5:2 by vol.) exhibits 58.50% capacity retention and 97.40% of the av. CE after 30 cycles with a cut-off voltage of 4.5 V at the charge and discharge current densities of 0.2 and 0.5 mA/cm2 at room temperature, respectively. Furthermore, 1 M LiPF6 in EA/FEC/TTE/EMC (2:1:5:2 by vol.) excellent cyclic performance in an MCMB‖NMC111 cell.

中文摘要    i
Abstract    iii
Acknowledgment    vii
Table of contents    ix
Index of figures    xiii
Index of tables    xxiii
Index of units and abbreviations    xxv
Chapter 1:     Introduction    1
1    Energy sources    1
2    Batteries as electrochemical energy storage systems    4
3    Lithium-based secondary rechargeable batteries    9
4    Electrolyte components for lithium-based rechargeable batteries    10
4.1    Solvents    11
4.2    Salts    13
Chapter 2:     The attraction of lithium and its challenge for Li-metal based batteries    15
1    Lithium metal batteries    15
2    Challenges in Li-metal based batteries    17
2.1    Reactivity of Li Metal    18
2.2    Volume changes in Li Metal    18
2.3    Growth of Li dendrites    20
2.4    The SEI on a Li metal anode    22
3    Engineering for stabilizing lithium metal batteries    23
3.1    Designing advanced electrolytes    24
3.2    Surface engineering on current collectors    24
3.3    Electrolyte additives    28
3.4    Artificial SEI engineering    33
4    Electrolyte chemistry for lithium metal batteries    34
4.1    Carbonate electrolytes    34
4.2    Ether-based electrolytes    35
4.3    High salt concentration electrolytes    36
4.4    Localized high concentration electrolytes    37
4.6    Fluorinated electrolytes    40
4.6    Single solvent and single salt electrolyte    41
5    Anode free lithium metal battery    43
6    Motivation and objectives of the study    51
6.1    Motivation    51
6.3    Objectives    53
Chapter 3:     Experimental section and characterization    55
1    Chemicals and reagents    55
2    Electrode fabrication    56
2.1    Cathode material    57
2.2    Anode current collector preparation    57
2.3    Electrolyte preparation    58
3    Physicochemical and flammability properties    59
4    Electrochemical measurement and characterization    60
4.1    Electrochemical measurements    60
4.2    Lithium morphology characterization    63
4.3    Surface composition characterization    63
4.4    Computational investigations    64
Chapter 4:     Dual electrolyte additives of potassium hexafluorophosphate and tris (trimethylsilyl) phosphite for anode-free lithium metal batteries    65
1    Introduction    65
2    Results and discussion    68
2.1    Li||Cu half-cell performance    68
2.2    Anode morphological evolution during cycling    71
2.3    Cu||NMC111 anode free full cells    73
2.4    Surface chemistry of the electrodes    80
4    Summary    85
Chapter 5:     Resolving the phase instability of a fluorinated ether, carbonate based electrolyte for the safe operation of anode-free lithium metal battery    87
1    Introduction    87
2    Results and discussion    90
2.1    Viscosity and conductivity measurements    90
2.2    Extended cycling performance of Cu||NMC111 using different electrolytes    93
2.3    Electrochemical stability and flammability test    101
2.4    Ionic conductivity and rate capability    104
2.5    Anode morphological evaluations of Li formed in situ on the Cu foil    107
2.6    Surface chemistry of the electrodes    108
2.7    Electrochemical performance of the MCMB||NMC111 full cell    111
3    Summary    115
 
Chapter 6:    Tolerance of low-temperature electrolyte for anode-free lithium metal battery    117
1     Introduction    117
2    Results and discussion    120
2.1    Viscosity and conductivity measurements    120
2.2    The wide temperature performance of electrolytes using Cu||NMC111    122
2.3    In situ plated lithium morphology on Cu substrate    131
2.5    Electrochemical performance of the MCMB||NMC111 full cell    133
3    Summary    134
Chapter 7:     Conclusions and future outlooks    135
1    Conclusions    135
2    Future outlooks    137
Reference    141
List of publication    171
Conference presentation    173


                                

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