鋰金屬與銅箔負極表面的介面物種生成研究｜國立臺灣科技大學博碩士論文系統

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研究生：	Bikila Nagasa Olana Bikila Nagasa Olana
論文名稱：	鋰金屬與銅箔負極表面的介面物種生成研究 Investigation of Formation of Solid electrolyte interphase over Lithium and Copper metal anode
指導教授：	林昇佃 Shawn D. Lin 黃炳照 Bing-Joe Hwang
口試委員:	She-Huang Wu She-Huang Wu Chun-Chen Yang Chun-Chen Yang Jyh-Chiang Jiang Jyh-Chiang Jiang Heng-Liang Wu Heng-Liang Wu
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：	2022
畢業學年度：	110
語文別：	英文
論文頁數：	150
中文關鍵詞：	Diffuse Reflectance Infrared Fourier-Transformed Spectroscopy 、Cyclic Voltammetry 、Energy- Dispersive X-ray Spectroscopy 、Open Circuit Potential 、Scanning Electron Microscopy 、X-ray photoelectron spectroscopy 、Zeolite imidazolate framework
外文關鍵詞：	Diffuse Reflectance Infrared Fourier-Transformed Spectroscopy, Cyclic Voltammetry, Energy- Dispersive X-ray Spectroscopy, Open Circuit Potential, Scanning Electron Microscopy, X-ray photoelectron spectroscopy, Zeolite imidazolate framework
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上一筆

在鋰金屬電池 (LMB)的鋰金屬陽極和無陽極 LMB (AFLMB) 的銅箔陽極表面，鋰枝晶和死鋰的形成是導致電池效能低落的主因。通過介面反應調控或施加人工塗層可能形成所謂的良好 SEI（固體電解質介面），可能會抑制電解質和電極之間的不良反應以及枝狀鋰的形成。本論文主要目的為研究在 OCV（開路電壓）下和初始迴圈期間，Li 和 Cu 金屬電極與電解質接觸時的表面物種形成現象，主要使用技術為原位 DRIFTS（漫反射紅外傅利葉變換光譜）分析。
第一項工作檢測電解質為LiTFSI (LiN(SO2CF3)2)溶在DME（1,2-二甲氧基乙烷）和 DOL（1,3-二氧戊環），並分析 LiNO3 (LN) 添加劑的影響。 OCV 下的 DRIFTS 光譜顯示Li 和 Cu 負極表面上的 DME 和 DOL是穩定的，而 LiTFSI 在 Li 負極上發生化學分解生成LiSO2CF3 和 Li2NSO2CF3 物種，但在 Cu 負極上是穩定的， LN則在 Li 和 Cu 陽極上化學分解成 LiNO2，以及可能的伴生物質 Li2O 。在 LSV（線性掃描伏安法），這些表面物質以及 DOL 和 DME 都會發生電化學還原，形成 ROLi（CH3CH2OCH2Li/CH3OCH2CH2OLi 和 CH3OLi，分別來自 DOL 和 DME）、Li3N（來自 TFSI- 和 LiNO3）、LiF 和 Li2SO2（來自TFSI-) 和 Li2O（來自 LiNO3）。
第二項工作氫氟醚 (TTE) 和環丁碸 (TMS) 溶解 LiTFSI的電解液(標記為 LiTT)，並分析 PS（多硫化鋰）添加劑的影響。 DRIFTS 分析顯示當TTE與鋰金屬接觸時，會分解生成 LiOCF2CF2H、LiCH2CFCFH 和 LiF 物質，TMS 與鋰金屬間反應形成 Li-C4H8SO2-Li，TFSI 離子則分解生成 LiSO2CF3 和 Li2SO2CF3 物質，這些OCV發生的反應，在浸沒測試和 XPS 分析中獲得佐證，並有證據顯示浸入時間較長時的碎片分解程度增加。 PS添加劑可以通過與鋰金屬優先反應形成Li2S和短鏈PS，可能鈍化表面抑制TTE、TMS和LiTFSI的分解。在 LSV 掃描時，LiSO2CF3 和 Li2NSO2CF3 物種可以還原為 LiCF3、Li2NO2Li、Li2SO2、LiF 和 Li3N。在帶有濺射金的Au/Cu陽極上，電解質的分解相較於 Li 金屬為低，在 Au/Cu 上形成的物質包括 LiSO2CF3 和 Li2NSO2CF3（來自 LiTFSI）、Li-C4H8-Li（來自 TMS）和LiOCF2CF2H 和 LiCH2CFCFH（來自 TTE）。
第三項工作中使用 LiTFSI/DOL-DME-LN 電解質檢查含有 ZIF8 (Zn(2-methylimidazolate)2) 覆層的銅箔陽極，並比較ZIF8中含有聚苯乙烯磺酸鹽 (PSS)的影響。具有Cu-ZIF8 和Cu-ZIF8-PSS覆層的陽極的可以提高電池長迴圈循環使用的穩定性，但初始庫侖效率相對裸Cu 陽極的電池為低。 DRIFTS 光譜顯示 SEI 物質仍然可以由電解質成分的還原反應而形成，SEM 和 EDX 分析顯示Cu表面可能沒有被 ZIF8 層完全覆蓋，這可能導致 SEI 的形成，並可能導致 ZIF8 覆蓋陽極之間的再現性有些不一致。
本研究的第四部份分析銅箔陽極上雙添加劑氟代碳酸亞乙酯 (FEC) 和二氟磷酸鋰 (LiPO2F2)對 SEI生成的協同作用，電解質為溶於碳酸亞乙酯 (EC) 和碳酸二乙酯 (DEC)的 LiPF6 。電解質成分在銅箔陽極上電化學還原反應，按照 LiPO2F2 > FEC > EC > DEC 的電位順序進行， LiPF6 在接觸 Cu 陽極時，有LixPFy生成，並在約 1.44 V時有還原反應。LiPF6 的還原物質會導致烷基氟化磷 (RPF) 的形成，不過這個反應會受到 FEC 和/或 LiPO2F2 的存在所抑制。FEC在第一個循環中還原並形成聚 (FEC)，而 EC 被電化學還原為 (CH2OCO2Li)2 和 Li2CO3，DEC被還原為 CH3CH2OCO2Li 和 Li2CO3。當僅使用 LiPO2F2 添加劑時，可以在 CV 中觀察到 LiPO2F2 的氧化還原現象，其中 LixPOy 作為可能的還原產物，使用LiPO2F2 可以減少Li2CO3 的形成，表明抑制了 EC 和 DEC 的還原。同時使用FEC 添加劑則可以抑制 LiPO2F2 的氧化還原作用，並可能通過 FEC 在 Cu 上的優先吸附來部分抑制 LiPF6 的分解。透過雙添加劑的電解質，顯示聚(FEC) 和 LixPFy 物種形成對LiPF6、EC 和 DEC 還原反應的抑制所帶來的可能優勢，但仍然無法完全抑制 LiPF6、EC 和 DEC 的還原。

In Lithium metal batteries (LMBs) with lithium metal anode and in anode-free LMBs (AFLMBs) with copper foil anode, formation of lithium dendrite and dead lithium is challenging. Formation of so-called good SEI (solid electrolyte interphase) by either in situ surface reaction or by prior artificial coating can possibly suppress undesired reactions between electrolyte and electrode, and dendritic lithium formation. The goal of this dissertation is to study surface species formation over Li and Cu metal electrodes upon contacting with electrolyte at OCV (open circuit voltage) and during initial cycles, by using in situ DRIFTS (diffuse reflectance infrared Fourier-transformed spectroscopy) analysis as the main technique.
In the first part, the electrolyte of LiTFSI (LiN(SO2CF3)2) in DME (1,2-dimethoxyethane) and DOL (1,3-dioxolane) with and without LiNO3 (LN) additive was examined. The DRIFTS spectra at OCV indicate the DME and DOL bands over Li and Cu anodes are similar and stable, while LiTFSI is chemically decomposed into LiSO2CF3 and Li2NSO2CF3 species over Li anode but it is stable over Cu anode. LN is chemically decomposed over both Li and Cu anodes into LiNO2 with Li2O as the likely accompanying species at OCV. During LSV (linear scan voltammetry) these surface species and also DOL and DME can be electrochemically reduced forming ROLi (CH3CH2OCH2Li/CH3OCH2CH2OLi and CH3OLi, respectively, from DOL and DME), Li3N (from TFSI- and LiNO3), LiF and Li2SO2 (from TFSI-), and Li2O (from LiNO3).
In the second part, the electrolyte of LiTFSI in hydrofluoroether (TTE) and sulfolane (TMS), labelled as LiTT, with and without PS (Lithium polysulfide) additive was investigated. DRIFTS analyses indicate that TTE decomposes into LiOCF2CF2H, LiCH2CFCFH and LiF species when in contact with lithium metal, and that TMS reacts with Li metal forming Li-C4H8SO2-Li. TFSI ion decomposition over Li leads to LiSO2CF3 and Li2SO2CF3 species at OCV. The chemical reactivity of Li toward all electrolyte components at OCV is supported by immersion tests and XPS analysis, with evidence of more fragmented species with longer immersion time. The PS additive can suppress the decomposition of TTE, TMS, and LiTFSI via preferential reaction with Li metal forming Li2S and short chain PS that may have passivated the surface. During LSV scanning LiSO2CF3 and Li2NSO2CF3 species can be reduced to LiCF3, Li2NO2Li, Li2SO2, LiF and Li3N. Over Cu anode with sputtered gold (Au/Cu), decomposition of electrolyte is relatively suppressed compared to over Li metal. The observed SEI species formed over Au/Cu include LiSO2CF3 and Li2NSO2CF3, (from LiTFSI), Li-C4H8-Li (from TMS), and LiOCF2CF2H and LiCH2CFCFH (from TTE).
In the third work, Cu anode coated with ZIF8 (Zn(2-methylimidazolate)2) layer with and without polystyrene sulfonates (PSS) was examined using LiTFSI/DOL-DME-LN electrolyte. The cell with Cu-ZIF8 and Cu-ZIF8-PSS anodes can improve long cycling stability though the initial coulombic efficiency is relatively low compared to cell with bare Cu anode. DRIFTS spectra indicate that SEI species still can be formed from reduced electrolyte components. SEM and EDX analyses indicate that Cu metal may not be completely covered by ZIF8 layer, which may contribute to SEI formation and somewhat inconsistent reproducibility among ZIF8-covered anodes.
The fourth work explores the possible synergetic effect of fluoroethylene carbonate (FEC) and lithium difluorophosphate (LiPO2F2) dual additives in SEI formation over Cu anode using LiPF6 in ethylene carbonate (EC) and diethyl carbonate (DEC). The electrolyte solvents and additives can be electrochemically reduced over Cu anode following a potential sequence LiPO2F2 > FEC > EC > DEC. LiPF6 interacts with Cu anode upon contact resulting in LixPFy which can be reduced at ~1.44 V. Without any additive, reduced species from LiPF6 can lead to formation of alkyl phosphorous fluorides (RPF) and this can be suppressed by the presence of FEC and/or LiPO2F2. When with only LiPO2F2 additive, redox of LiPO2F2 can be observed in CV with LixPOy as the possible reduced product. In addition, Li2CO3 formation from EC and DEC reduction was relatively suppressed by the presence of LiPO2F2. The simultaneous presence of FEC additive can suppress the redox of LiPO2F2 and partly the decomposition of LiPF6 likely via preferential adsorption of FEC on Cu. The electrolyte with dual additives demonstrates a possible advantage from poly(FEC) and LixPOy species formation, resulted in suppressed reduction though not completely of LiPF6, EC and DEC.

Abstract    i
Acknowledgement    v
List of Figures    x
List of Scheme    xvii
Chapter 1: Introduction    1
1.    Lithium Metal Anode    1
2.    Solid Electrolyte Interphase Formation    2
3.    Modifying Copper anode with artificial SEI.    7
4.    Techniques of SEI analysis    7
5.    Motivation and Aim of the current work.    11
Chapter 2: Experimental methods    13
1 Electrolyte preparation    13
1.1 Lithium bis(trifluoroethane)sulfonimide in DME: DOL    13
1.2 Lithium bis(trifluoroethane)sulfonimide in TMS: TTE    13
1.3 LiPF6 in ethylene carbonate (EC): diethyl carbonate (DEC)    14
2 Electrode preparation    14
3 Electrochemical Measurement    15
3.1 CV, EIS and Charge Discharging Experiment    15
4 FTIR and DRIFTS Experiment    15
5. XPS, Raman, SEM image and EDX analysis    16
Chapter 3: In Situ DRIFTS study of solid electrolyte interphase formation on Lithium metal anode from ether based LiTFSI with and without Lithium nitrate and fluoropyridine additives.    17
1 Motivation    17
1    Results and discussion    18
1.1    Electrochemical performances of Li||Li and Cu||Li cells    18
1.2    Electrochemical impedance spectroscopy Measurement    20
1.3    Cyclic voltammetry Measurement    22
1.4    In situ DRIFTS over Li and Cu electrodes at OCV.    24
1.5    In Situ DRIFTS difference spectra over Li metal anode during electrochemical cycling    …………………………………………………………………………………………28
1.6    In Situ DRIFTS difference spectra over Cu anode during electrochemical cycling    …………………………………………………………………………………………33
1.7    X-ray photoelectron spectroscopy    37
1.8    Scanning electron microscope images of electrodes after cycling    40
4.    Summary    44
Chapter 4: Chemical reaction between LiTFSI in TMS-TTE electrolyte with Li metal anode    45
1 Motivation    45
2 Results and Discussion    46
2.1 FTIR analysis of Liquid Samples    46
2.2 DRIFTS analysis of TMS and TTE solvents over Li    48
2.3 DRIFTS analysis of LiTT and LiTT-PS electrolyte over Li    51
2.4 X-ray photoelectron spectroscopy analyses    56
2.5 FTIR/DRIFTS difference spectra    60
2.6 Comparison of in situ DRIFTS spectra over Li and Au/Cu electrodes at OCV    63
2.7 Cyclic voltammetry Measurement    65
2.8 EIS Measurement    68
2.9 In situ DRIFTS difference spectra during electrochemical cycling    69
2.10 Raman spectra analysis of electrode after cycling    75
2.11 X-ray photoelectron spectroscopy results    77
3 Summary    81
Chapter 5: Improving long cycling performance of copper anode using ZIF8 artificial film.    82
1 Motivation    82
2 Results and discussions    83
2.1 DRIFTS characterization of Cu anode coated with ZIF8 and ZIF8-PSS    83
2.2 SEM, cross-sectional FIB image and EDX elemental mapping of Cu-ZIF8 and Cu-ZIF8-PSS electrodes.    84
2.3 Cyclic Voltammetry Measurement    86
2.4 In situ DRIFTS spectrum over Cu-ZiF8 and Cu-ZiF8-PSS anode using LiTFSI in DME/DOL with LiNO3 electrolyte    88
2.5 Electrochemical Performance Measurement.    92
2.6 EIS Measurement    95
2.7 Top view SEM, cross-sectional FIB image and EDX/elemental mapping of anode after
cycling.    98
3 Summary    102
4 Comparison of SEI formed over Li and Cu metal anodes    103
Chapter 6: In Situ Diffuse Reflectance Infrared Fourier Transform Spectroscopy Investigation of Fluoroethylene Carbonate and Lithium Difluorophosphate Dual Additives in SEI Formation Over Cu Anode.    105
1 Motivation    105
2 Results    106
2.1 Cyclic voltammetry Measurement    106
2.2 In situ DRIFTS at OCV    108
2.3 In situ DRIFTS difference spectra using LP47 base electrolyte    111
2.4 In situ DRIFTS spectra of LP47 with FEC additive    113
2.5 In situ DRIFTS spectra of LP47 with LiPO2F2 additive    115
2.6 In situ DRIFTS spectra of LP47 with FEC and LiPO2F2 dual additive    116
3 Summary    121
Chapter 7: General conclusion    123
Chapter 8: Recommendation and Future prospective.    126
References    127
Appendices    145


                                

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