固態硫化物和液態電解質中的界⾯電化學⽤於鋰⾦屬電池

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研究生：	Bereket Woldegbreal Taklu Bereket Woldegbreal Taklu
論文名稱：	固態硫化物和液態電解質中的界⾯電化學⽤於鋰⾦屬電池 Interface Electrochemistry in Solid Sulfide and Liquid Electrolyte for Lithium Metal Batteries
指導教授：	蘇威年 Wei-Nien Su 黃炳照 Bing-Joe Hwang
口試委員:	劉如熹 Ru-Shi Liu 張仍奎 Jeng-Kuei Chang 王迪彥 Di-Yan Wang 吳溪煌 She-Huang Wu
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2023
畢業學年度：	111
語文別：	英文
論文頁數：	264
中文關鍵詞：	全固態電池、鋰硫銀鍺礦、⿄化物固態電解質、熏碘、鋰⾦屬相容性、鋰枝晶抑制、離⼦電導率、實際電化學窗⼝、⽔分穩定性、氣體摻雜、多重SEI形成、界⾯化學、熱解、成本效益、原位光學顯微鏡測量、原位拉曼光譜
外文關鍵詞：	All-solid-state batteries, Lithium argyrodite, Halide solid electrolyte, Fumy iodine, Lithium-metal compatibility, Dendrite suppression, Ionic conductivity, Practical potential window, Moisture stability, Gas doping, Multiple SEI formation, Interface chemistry, Thermal pyrolysis, Cost effective, In-situ optical microscopic measurement, In-situ raman spectroscopy
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近年來，全固體鋰金屬電池因其兼具高能量密度與安全性等優點而逐漸受到關注，而Li-argyrodite硫化物固態電解質具有優秀的延展性、高導離、低成本、多樣的合成方法等優勢在全固態電池的應用中嶄露頭角。其與"聖盃"鋰金屬陽極搭配更是實現固態與液態電池卓越能量密度的關鍵，與傳統的鋰金屬、鋰離子電池相比，全固態鋰金屬電池在高能量電網與電動汽車的應用上，更有潛力帶來革命性的發展進化。
Li-argyrodite硫化物固態電解質因諸多優良特性在全固態鋰金屬電池中備受矚目，但其與鋰金屬陽極界面卻有嚴重的不相容性，鋰枝晶的雜亂生長與氣相不穩定性阻礙了其應用，因此，我們提出了一種無球磨的CuCl雙摻雜合成法來克服此問題，將CuCl摻雜於Li-argyrodite硫化物超導體 (Li6+3xP1-xCuxS5-xCl1+x)中，以複合電極與平面電極對此Li6.3P0.9Cu0.1S4.9Cl1.1 (LPSC-1)進行測試，室溫下Li+離子最大導離率可達4.34 mS cm-1且具有極佳的電壓穩定性8 V vs. Li/Li+，此外，經測試在50 °C下以3 mA cm-2的電流密度進行測試後發現，其亦能抑制鋰枝晶的生長。在0.1與1 mA cm-2的電流密度下進行對稱電池循環測試，此電解質在超過2400小時與400小時的測試中幾乎沒有發現過電位的產生，表示出其顯著的可逆性。後使用XPS與交流阻抗分析證明此方法確實有效的增進了鋰金屬與固態電解質間的介面穩定性，且實現了3 mA cm-2的臨界電流密度，更有趣的是，我們發現將此Li6.3P0.9Cu0.1S4.9Cl1.1 (LPSC-1)與軟酸Cu結合後，其空氣穩定性獲得了提升且將H2S的生成降低至原先的1/2，最後，將LPSC-1暴露於空氣前後的XRD證實了此硫化物固態電解質的確實降低了親氧性。
在我們第二項工作中，我們提出一款碘化氯氧化的argyrodite，此碘化氯氧化的argyrodite在充放電時能同時形成含有堅固LiI與Li2O的SEI，這能有效的緩解阻抗界面的增長、提升氧化穩定性、降低氧親合力。此外，藉由犧牲碘產生的誘導效應，我們實現了10mA cm-2的高臨界電流密度，而在截止電容高達10 mAh cm-2與10 mA cm-2的電流密度條件下測試260小時發現，其具有超高鋰兼容性，耐久度測試方面，分別以0.1、2、6 mA cm-2的電流密度循環11000、1000、460 小時進行測試，且從逐步CV的結果我們可以得知，實際電化學窗口的穩定性提升至了3.42 V vs. Li/Li+。以Li6PS4.8O0.2Cl-5 wt% I2搭配鋰銦陽極的條件下，分別進行1C與3C的充放電測試，在200圈與300圈後個別電容保持率可達89.6%與89.9%，在0.4C下發現，其與鋰金屬具有極為優異的循環穩定性且初始放電電容量達137.27 mAh g-1，最後，通過耦合原位拉曼量測證實，其提升了與水的耐受性並抑制了H2S氣體的生成。
在最後的工作中，我們發表了一款新型人造鈍化層來穩定鋰金屬，藉由NH4F鹽類的熱解反應來產生HF(g)與NH3(g)，利用"聖盃"鋰金屬的熱力學不穩定性與會生長枝晶的特性，將其暴露在NH4F鹽類生成的氣體中即可產生自發反應，形成與NH4F鹽類相關的多種成分的SEI如: LiF、Li3N、Li2NH、LiNH2、與LiH等。這種表面上含有人工保護層的鋰金屬(AF-Li) ，在Li||Li對稱電池中可以持續穩定鋰的沉積與剝離，減少枝晶的生成；而在Li||Cu與Li||MCMB等半電池系統中，我們更進一步闡述此膜優異的保護特性，此外，其與正極氧化物間具有相當好的相容性、展示了相當優異的電容維持率，與LFP在0.5 mA cm-2的電流密度下循環280圈後CR仍有90.6%、與NMC532在3 mA cm-2的電流密度下循環410圈後CR仍有58.7%。重要的是，使用此款NH4F鹽類生層的人造層能同時間生成多種成分的SEI，且製程簡便、價格具競爭力，這使得其在眾多改良方法中極具競爭力。

All-solid-state lithium metal batteries, with ultimate safety and high energy density, are receiving increasing attention. The Li-argyrodite sulfide solid electrolyte, with decent ductility, high ionic conductivity, low cost, and versatility in synthesis methods, shows promise for use in all-solid-state lithium batteries. Integration with the "Holy Grail" lithium metal anode is pivotal in achieving superior energy density in both solid and liquid electrolyte systems. All-solid-state lithium metal batteries have the potential to revolutionize high grid and EV use when compared to traditional LMBs and LIBs in the near future.
The Li-argyrodite sulfide solid electrolyte with versatile properties makes promising for all-solid-state lithium metal batteries. However, its serious interfacial incompatibility with Li anode, dendrite growth, and intrinsic air instability impedes its practicability. Herein, we report a CuCl dual doped Li-argyrodite sulfide superb-conductor (Li6+3xP1-xCuxS5-xCl1+x) prepared to overcome these issues via ball-mill free synthesis approach. The maximum Li+ conductivity of 4.34 mS cm-1 at room temperature with ultrawide voltage stability up to 8 V vs. Li/Li+ was achieved in Li6.3P0.9Cu0.1S4.9Cl1.1 (LPSC-1) via a both composite and planar electrode system and can suppress dendrite formation at a current density of 3 mA cm-2 at 50 оC. The symmetrical cell cycled at 0.1 and 1 mA cm-2 also demonstrates remarkable reversibility with negligible overpotential alteration for more than 2400 h and 400 h. An ex-situ XPS and AC impedance analysis proved enhanced interfacial compatibility at Li | SE and achieved a critical current density of 3 mA cm-2. More interestingly, incorporating soft acid Cu in LPSC-1 boosts the air stability and suppresses H2S generation by two-folds. The XRD for the LPSC-1 before and after air exposure proves the decrease in the oxophilicity of the sulfide solid electrolyte.
In our second work, we report iodized-oxychloride argyrodite with robust SEI containing in-situ formed LiI and Li2O upon treating the sulfide via fumy iodine to mitigate the growth of resistive interphase, limited oxidative stability, and highly-oxophilic nature of sulfide solid electrolyte. Sacrificial iodine-induced dendrite suppression capability up to 21 mA cm-2 was achieved. Ultrahigh-lithium compatibility with a high cutoff-capacity of 10 mAh cm-2 was cycled at 10 mA cm-2 for 260 h. Moreover, durable cycling was performed at 0.1 mA cm-2 for 11000 h, 2 mA cm-2 for 1000 h, and 6 mA cm-2 for 460 h. Stepwise CV measurement demonstrates enhanced “True practical potential window” stability up to 3.42 V vs. Li/Li+. Cell performance of Li6PS4.8O0.2Cl-5 wt% I2 with Li-In at 1 C and 3 C has achieved capacity retention of 89.6 % and 89.9 % after 200 and 300 cycles. Outstanding cyclability with Li-metal at 0.4 C with an initial-discharge capacity of 137.27 mAh g-1 was achieved. Enhanced tolerance to moisture with suppressed H2S gas generation was proven by coupling in-situ Raman measurements.
In the final work, we report a novel artificial stabilization of lithium metal was carried out via the thermal pyrolysis of NH4F salt, which generates HF(g) and NH3(g). The use of the "Holy Grail" lithium metal anode faces practical challenges originating from thermodynamic instability of lithium metal and dendrite growth. Herein, an exposure of lithium metal to the generated gas induces a spontaneous reaction that leads to the formation of multiple SEI components, such as LiF, Li3N, Li2NH, LiNH2, and LiH, from a single salt. The artificially protected layer on lithium metal (AF-Li) sustains stable lithium stripping/plating and endures Li dendrite under Li||Li. The half-cell Li||Cu and Li||MCMB systems depicted the attributions of the protective layer. We demonstrate the treasure of AF-Li, coupled with the oxide cathode, delivered outstanding capacity retention (CR). LFP showed a CR of 90.6% at 0.5 mA cm-2 after 280 cycles, and NCM523 showed a CR of 58.7% at 3 mA cm-2 after 410 cycles. The formulation of the artificial protective layer, with simultaneous formation of multiple SEI components, is facile and cost-effective from NH4F as a single salt, making the system competent.

中文摘要………    i
Abstract.………    iv
Acknowledgment    vii
Table of contents    ix
List of figures…    xiii
List of units and abbreviations    xxxiii
Chapter 1: Introduction    1
1    Energy source and renewability    1
2    Electrochemistry of lithium batteries    6
Components in electrochemical cells    8
3.1    Electrode    8
3.2    Separator    8
3.3    Electrolyte    9
3.4    Current collectors    12
Chapter 2:  All solid-state lithium metal batteries and its challenges    13
1    Solid electrolyte superconductors    13
2    Advantages of all solid-state lithium batteries    15
2.1    Safety    15
2.2    Energy density    15
2.3    Cycle life    16
3    Challenges in solid-state lithium batteries    16
4    Categories of sulfide solid electrolyte    18
4.1    Glasses    19
4.2    Glass-ceramic    20
4.3    Thio-LISICON    20
4.4    LGPS-type    21
4.5    Argyrodite type    21
5    Ion-transport mechanisms in solid electrolyte    22
5.1    Polymer electrolytes    22
5.2    Inorganic solid electrolytes    24
6    Synthesis approach in sulfide solid electrolyte    28
6.1    Solid-state synthesis    29
6.2    Solution / liquid-based synthesis    30
6.3    Mechanical synthesis    32
7    Electrochemical potential window stability    33
8    Interfacial phenomena at electrode / solid-electrolyte interface    34
8.1    Cathode electrolyte interface and chemomechanical properties on cell performance    34
8.2    Anode-electrolyte interface    36
9    Dendrite growth and propagation mechanism in SSE    38
10   Gas phase lithium metal treatment for lithium metal batteries    41
11   Hydrolysis of sulfide solid electrolyte and moisture stabilization approaches    42
12    Motivation and objectives of the study    48
12.1    Motivation    48
12.2    Objectives    49
Chapter 3:  Experimental section and characterization    51
1    Chemicals and reagents    51
2    Electrode fabrication    52
3    Solid electrolyte synthesis and optimization conditions    53
3.1    Dual CuCl doped argyrodite sulfide synthesis and optimization conditions    54
3.2    Oxygen doped argyrodite sulfide synthesis and optimization    55
3.3    Synthesis of oxygen doped-iodized argyrodite sulfide and optimization conditions    56
4    Moisture stability and hydrogen sulfide (H2S) measurement    58
5    Computational details for lithium/sulfide solid electrolyte interface chemistry    60
6    Gas phase treatment of lithium metal anode    60
7    Characterizing techniques    61
7.1    Structural analysis via XRD diffraction    62
7.2    Structural analysis via Raman spectroscopy    63
7.3    Morphological characterization    64
7.4    Surface chemistry and compositional analysis    65
8    Electrochemical characterization techniques    66
8.1    Electrochemical Impedance Spectroscopy    66
8.2    Cyclic voltammetry and linear sweep voltammetry    67
8.3    Galvanostatic charge-discharge cell performance    68
Chapter 4: Dual CuCl doped argyrodite superconductor to boost the interfacial capability and air stability of all solid-state lithium metal batteries    71
1    Introduction    71
2    Results and discussion    73
2.1    Structure characterizations of sulfide solid electrolytes    73
2.2    Effect of CuCl dual doping ionic conductivity and lithium diffusivity    79
2.3    Practical electrochemical potential window    83
2.4    Lithium compatibility and dendrite suppression in sulfide solid electrolyte    87
2.5    Interface chemistry and post-mortem analysis    98
2.6    Moisture stability and structural alterations    101
3    Summary    104
Chapter 5:  Air-stable iodized-oxychloride argyrodite sulfide and anionic swap on the practical potential window for all-solid-state lithium-metal batteries    107
1    Introduction    107
2    Results and discussion    110
2.1    Structural characterization of Li6PS5-xOxCl and Li6PS4.8O0.2Cl-y wt% I2    110
2.2    Ionic conductivity and optimation conditions    112
2.3    Practical electrochemical potential window of sulfide solid electrolytes    116
2.4    Lithium compatibility and dendrite suppression capability    124
2.5    Surface chemistry of sulfide solid electrolytes    138
2.7    Electrochemical cell performance    144
2.8    Moisture stability and compositional alteration via in-situ Raman measurement    147
3    Summary    151
Chapter 6:    Mechanistic study on artificial stabilization of lithium-metal anode via thermal pyrolysis of NH4F in lithium metal batteries    153
1    Introduction    153
2    Results and discussion    154
2.1    Reaction mechanism and structural material characterizations    154
2.2    Artificial lithium protection and suppression of lithium dendrite    159
2.3    Half-cell electrochemical performance with Cu and MCMB substrate    163
2.4    Electrochemical performance in full-cell configurations    170
3    Summary    174
Chapter 7: Conclusions and future outlooks    175
1    Conclusions    175
2    Future outlooks    178
References…….    181
List of publication    218
Conference presentation    221
Appendix..……..    222
                                

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全文公開日期 2026/07/17 (校內網路)
全文公開日期 2026/07/17 (校外網路)
全文公開日期 2026/07/17 (國家圖書館：臺灣博碩士論文系統)

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