以界面工程改善無陽極鋰電池壽命｜國立臺灣科技大學博碩士論文系統

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研究生：	Niguse Aweke Sahalie Niguse Aweke Sahalie
論文名稱：	以界面工程改善無陽極鋰電池壽命 Cycle Life of Anode-Free Lithium Metal Battery Improved by Interfacial Engineering Approaches
指導教授：	黃炳照 Bing-Joe Hwang 蘇威年 Wei-Nien Su
口試委員:	吳溪煌 She-Huang Wu 鄧熙聖 Hsisheng Teng 林律吟 Lu-Yin Lin 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：	2020
畢業學年度：	108
語文別：	英文
論文頁數：	224
中文關鍵詞：	鋰金屬電池、無陽極、硝酸鉀添加劑、固液界面膜的形成、屏蔽效果、三元系陰極、庫侖效率、氧化鋁/聚丙烯腈、潤濕性、親鋰性、鋰枝晶抑制
外文關鍵詞：	Li metal battery, anode free, KNO3 additive, SEI formation, shielding effect, NMC, coulombic efficiency, Al2O3/PAN, wettability; lithophilicity, LAP film, dendrite suppression
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在過去的幾十年中，鋰離子電池（LIB）已經成為替代能源需求的替代品。高能量密度，充放電速率，長循環壽命和低自放電是在不同攜帶式電子設備中使用的LIB的幾個重要特徵。但是，商用LIB仍無法為電動汽車和大型儲能裝置提供足夠的能量。鋰金屬陽極因其高理論電容（3860mAh g-1）、低還原電位（-3.04V vs SHE）和低密度（0.534g cm-3）在最近被受到重視。
使用無陽極組裝的無陽極鋰金屬電池（AFLMB）可以顯著提高電池的能量密度成本和安全性。因此, AFLMB採用從預置鋰到銅電流收集器的可逆提取鋰的方法。然而，鋰陽極和AFLMB都會遇到不穩定的鋰電鍍/剝離過程。鋰在銅電極上的不均勻沉積會導致枝晶生長、SEI積累、庫侖效率低和循環壽命短。因此，本論文採用幾種方法來解決鋰金屬陽極和AFLMB的障礙。
第一種方法是基於雙功能電解質添加劑的使用。研究硝酸鉀（KNO3）添加劑對AFLMB全電池（Cu ǁ LiNi1/ 3Mn1 / 3Co1 / 3O2或Cu ǁ NMC）和半電池（Cu ǁ Li）構型的循環壽命和平均庫侖效率（CE）的影響。Cu ǁ NMC電池在有KNO3的情況下, 經過50次循環後的電容保持率（CR）約為40%，對照電解質，1 M LiPF6在碳酸亞乙酯（EC）和碳酸二乙酯（DEC）（1:1 v/v）中，的15個循環後，其電容保持率（CR）為40%。含添加劑的Cu ǁ NMC電池50次循環的平均CE增至96.50%，而無KNO3的35次循環後的平均CE為91.32%。在有無KNO3的60個循環後，Cu ǁ Li電池的平均效率分別為96.20%和85.74%。掃描式電子顯微鏡（SEM）的形態學研究表明, KNO3可使鋰沉積相對平滑。這些結果主要來自（1）PF6–和 NO3–的還原作用增強新的固體-電解質界面組成，以及（2）K+的靜電屏蔽作用。
第二項工作是在銅電極表面塗布研磨的Al2O3 /聚丙烯腈（PAN）複合層（AOP）的效果。Cu上的AOP層可促進從NMC（333）陰極提取的緻密且平滑的Li沉積，從而延長循環壽命。 AOP層的優異潤濕性和電解質吸收特性促進了均勻的離子通量和相應的電化學動力學。多功能AOP層為SEI層提供了適度的機械支撐，同時還提供了足夠的強度來抑制鋰枝晶的生長。從AOP的底部在負極表面形成Li–Al–O/Al2O3的物質揭示了複合層的親鋰性質，通過調節Li+通量，除了Al–F外，還形成了新的SEI組成。PAN協同作用通過其靈活的結合作用和對鋰通量具有良好親和力的氮的存在來體現。所得的帶有AOP@Cu的電池如AOP@Cu ǁ NMC（333）和AOP@Cu ǁ Li電池改善的循環穩定性和庫侖效率。在0.2 mA cm-2下進行的AOP @Cu ǁ NMC（333）電池具有160 mAh g-1的第一循環放電電容，在82次循環後仍保持30%，而Cu ǁ NMC電池從146.31 mAh g-1的第一循環放電電容經過52次循環後仍保持約30%。
最後一種方法透過LAP層修飾Cu電極，該層是透過將LiNO3奈米粒子摻入Al2O3/PAN複合材料（AOP）主體中製成的。主體的膜受益於復合組成的協同作用。聚合物（PAN）用作黏合劑和Li+通量調節劑，而復合LAP機械支撐形成的固體-電解質界面（SEI）。LAP複合層可提供更好的潤濕性，還可透過界面孔吸收電解質，從而產生均勻的鋰通量。奈米級摻入的LiNO3一部分釋放到電解質中，並改善了電荷轉移動力學。它還經過還原分解以形成更好的SEI組成，包括Li3N和LiNxOy，從而獲得更好的導電性和更少的極化電池。因此，獲得了無枝晶且平滑的鋰沉積。與相應的對照電池相比，LAP@Cu ǁ Li和LAP@Cu ǁ NMC電池可提供更好的電容保持能力和庫侖效率。LAP@Cu ǁ NMC電池在0.5 mA cm-2下進行，含有10%FEC電解質添加劑，在140次循環後仍保持第一循環放電電容的30%。在250和100次循環後，LAP@Cu ǁ Li電池的平均庫侖效率（CE）分別在0.5 mA cm-2、0.5 mAh cm-2和1 mA cm-2、1 mAh cm-2為98.16%和99.37%。
大部分情況下，使用電解質添加劑和表面塗層的界面工程方法可以增加AFLMB的循環壽命。由硝酸鹽還原形成良好SEI成分的硝酸鉀電解質添加劑可穩定鋰沉積和剝離的過程。相較於鋰離子相比，還原電位最低的陽離子鉀產生的靜電屏蔽機制進一步穩定了加工並延長了電池的循環壽命。通過AOP和LAP複合層進行表面塗層還可以提高SEI的強度，增加潤濕性並調節鋰離子沉積。此外，作為LAP摻入薄膜中的鹽可以穩定釋放到電解質中，所形成SEI效果優於單獨使用硝酸鉀和AOP的方法。

Over the last decades, the lithium-ion batteries (LIB) have appeared as an alternative to the
increasing demand of energy source. The high energy density, rate of charge and discharge, reliability, and low self-discharge are some of the important features of LIB to be utilized in different portable electronic devices. However, the commercial LIB cannot still deliver enough energy for electric vehicles and large scale storages. Recently, lithium metal anode got a great attention due to its high theoretical specific capacity (3860 mAh g 1), lowest reduction potential (-3.04 V vs SHE) and lowest density (0.534 g cm-3).
Utilizing anode free Lithium metal battery (AFLMB) which is assembled without any anode could significantly increases the energy density, cost and safety of a cell. AFLMB is therefore adopts the reversible extraction of lithium (Li) from prelithiated cathode on to Cu current collector. Nevertheless, both lithium anode and AFLMB suffers from unstable lithium plating/stripping process. The uneven Li deposition on copper current collector results in dendrite growth, SEI accumulation, low coulombic efficiency and short cycle life. Therefore, in this thesis, several approaches have been undertaken to solve the hurdles in lithium metal anode and AFLMB.
The first approach is based on the use of bifunctional electrolyte additive. The effect of potassium nitrate (KNO3) additive to boost the cycling life and average coulombic efficiency (CE) of both AFLMB full cell (CuǁLiNi1/3Mn1/3Co1/3O2 or CuǁNMC) and half cell (CuǁLi) configurations is studied. The CuǁNMC cell possesses a capacity retention (CR) of ~40% after 50 cycles in the presence of KNO3 compared to ~40% after 15 cycles in the control electrolyte, 1 M LiPF6 in ethylene carbonate (EC) and diethyl carbonate (DEC) (1:1 v/v). The average CE of CuǁNMC cell with additive for 50 cycles increases to 96.50%, whereas it is 91.32% after 35 cycles without KNO3. The average efficiencies of CuǁLi cells are 96.20% and 85.74% after 60 cycles with and without KNO3 respectively. Morphological investigations by Scanning Electron Microscope (SEM) reveal a relatively smooth Li deposition with KNO3. These achievements originate mainly from (1) new solid electrolyte interphase components from the enhanced reductive decompositions of PF6– and NO3– and (2) electrostatic shielding effect of K+.
The second work is on the effect of milled Al2O3/Polyacrylonitrile (PAN) composite layer (AOP) coated on the surface of Cu current collector. AOP@Cu layer encourages compact and smoother Li+ deposition, extracted from NMC (333) cathode, for better cycle life. The excellent wettability and electrolyte uptaking nature of AOP layer promotes uniform ionic flux and the corresponding electrochemical kinetics. Multifunctional AOP layer offers a moderate mechanical support to the SEI layer, while it also provides sufficient strength to suppress the growth of lithium dendrites. The formation of Li – Al – O/Al2O3 species from the bottom part of AOP at the negative electrode surface reveals the lithiophilic nature of the composite layer to form new SEI components, in addition to Al – F, by regulate Li+ flux. PAN synergism is manifested by its flexible binding role and by the presence of nitrogen that has good affinity to lithium flux. The resulting cell with AOP@Cu possesses improved cycling stability and Coulombic efficiency in AOP@CuǁNMC (333) and AOP@CuǁLi cells. AOP@CuǁNMC (333) cell run at 0.2 mA cm-2 exhibits a first cycle discharge capacity of 160 mAh g-1 which retains 30% after 82 cycles, while CuǁNMC cell retains ~30% after only 52 cycles from the first discharge capacity of 146.31 mAh g-1.
The last approach involves the modification of Cu current collector by LAP layer which is fabricated by incorporating of LiNO3 into the Al2O3/PAN composite (AOP) host. The host film benefits from the synergetic effect of composite components. The polymer (PAN) acts as a binder and Li+ flux regulator while the composite LAP mechanically supports the as formed solid electrolyte interphase (SEI). LAP composite layer provides better wettability and also electrolyte uptake through interfacial holes that result in uniform Li flux. The incorporated LiNO3 partly released into the electrolyte, and improve the charge transfer kinetics. It also undergoes reductive decomposition to form better SEI components including Li3N and LiNxOy resulting better conductive and less polarized cell. Consequently, dendrite free and smooth lithium deposition was obtained. The LAP@CuǁLi and LAP@CuǁNMC cells deliver far better capacity retention and coulombic efficiencies than the corresponding control cells. The LAP@CuǁNMC cell run at 0.5 mA cm-2 with 10% FEC electrolyte additive retains 30% of the first discharge capacity after 140 cycles. The average coulombic efficiency (CE) of LAP@CuǁLi cell is also 98.16% at 0.5 mA cm-2, 0.5 mAh cm-2 after 250 cycles and 99.37% at 1 mA cm-2, 1mAh cm-2 after 100, cycles respectively.
Generally, interfacial Engineering approaches by using electrolyte additives and surface coating can enhance the cycle life of AFLMB. KNO3 Electrolyte additives that form good SEI components from nitrate reduction stabilize the plating/stripping process. Electrostatic shielding mechanism by cations, K+, with lowest reduction potential than Li+ further stabilizes the processes and enhance the cycle life of the cell. The effects of surface coating by AOP and LAP composite layer can also mechanically support the SEI, increases the wettability and regulate the Li+ deposition processes. In addition, salts incorporated into the film as LAP could be steadily released into the electrolyte to form SEI components which performs better than KNO3 and AOP approaches done separately.

摘要    i
Abstract    v
Acknowledgment    viii
Table of Contents    xi
List Abbreviations and Units    xxiv
Chapter 1: Introduction    1
1.    Backgrounds of energy sources    1
2.    Batteries as electrochemical energy storage    3
3.    Lithium secondary battery    4
3.1.    Cathode materials    6
3.2.    Anode materials    10
3.3.    Electrolytes    13
3.4.    Electrolyte additives and solid electrolyte interphases    17
3.5.    Separator    19
3.6.    Interfacial Engineering    21
4.    Anode-free lithium metal battery    22
Chapter 2: Understanding and improving the cyclability of lithium metal anode and anode-free battery    25
1.    Lithium metal as anode    25
2.    Conventional challenges in lithium metal anode    26
2.1.    Dendrite growth and its consequences    27
3.    Approaches to enhance the cycle life of lithium metal anode    32
3.1.    Electrolyte Engineering    33
3.2.    Electrolyte additives    37
3.3.    Solid electrolytes    40
3.4.    Surface Engineering    44
3.5.    Separator Engineering    50
3.6.    Controlling the charge-discharge parameters    51
4.    The progress of anode free lithium metal battery    53
5.    Motivation and objectives of the study    57
5.1.    Motivation    57
5.2.    Objectives    58
Chapter 3: Materials and experimental methods    59
1.    Chemicals and reagents    59
2.    Experimental section    60
2.1.    Preparation of KNO3 containing electrolyte    60
2.2.    Electrolyte characterization    60
2.3.    Electrode preparation    61
2.4.    Fabrication of AOP coated Cu (AOP@Cu)    61
2.5.    Characterization of AOP layer    63
2.6.    Fabrication of LiNO3/Al2O3/PAN coated Cu (LAP@Cu)    63
2.7.    Characterization of LAP layer    65
2.8.    Electrochemical measurements    65
2.9.    Physicochemical characterization of SEI    66
Chapter 4: Effect of bifunctional additive potassium nitrate on performance of anode free lithium metal battery in carbonate electrolyte    67
1.    Introduction    67
2.    Results and discussion    70
2.1.    Electrolyte and electrode preparation    70
2.2.    Morphology of Li electrodeposited onto Cu    71
2.3.    Electrochemical cycling stability    74
2.4.    Analysis of surface chemistry    83
3.    Summary    90
Chapter 5: Multifunctional properties of Al2O3/polyacrylonitrile composite coating on Cu to suppress dendritic growth in anode free Li-metal battery    93
1.    Introduction    93
2.    Results and discussions    97
2.1.    AOP@Cu preparation and characterization    97
2.2.    Morphology of deposited Li metal    100
2.3.    Electrochemical performance    105
3.    Summary    117
Chapter 6: Manipulating solid electrolyte interphase through selective reduction of nano-dispersed salt in ceramic artificial layer for anode free lithium metal battery    119
1.    Introduction    119
2.    Results and discussion    122
2.1.    Fabrication of LiNO3/Al2O3/PAN coated Cu (LAP@Cu)    122
2.2.    The effect of LAP on Li growth morphology    124
2.3.    Electrochemical performances    126
3.    Summary    139
Chapter 7 Conclusion and future perspectives    143
1.    Conclusion    143
2.    Future perspectives    145
Appendixes    191
Approach I    191
Approach II    192
Approach III    194


                                

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