透過臨場與原位光譜影像技術探索電化學能源材料｜國立臺灣科技大學博碩士論文系統

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研究生：	黃貞睿 Chen-Jui Huang
論文名稱：	透過臨場與原位光譜影像技術探索電化學能源材料 Exploring Electrochemical Energy Materials by in-operando/situ Spectroscopy and Imaging Techniques
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 吳乃立 Nae-Lih Wu 鄧熙聖 Hsisheng Teng 楊純誠 Chun-Chen Yang 張仍奎 Jeng-Kuei Chang
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：	163
中文關鍵詞：	臨場與原位光譜影像技術、金屬電池、鋰硫電池、無陽極鋰金屬電池、水系鋅金屬電池、反應機制、金屬沉積溶解行為、充放電機制
外文關鍵詞：	-situ/operando spectroscopy and imaging techniques, metal battery, Li-S battery, anode-free Li-metal batteries, aqueous Zn-metal battery, reaction mechanism, metal deposition/stripping, charge/discharge mechanism
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上一筆

近年來，隨著快速發展的電動車、穿戴式電子裝置與3C電子產品，對於儲存的需求也跟著與日俱增。然而，現今商業化鋰離子電池已逐漸達到其理論能量密度與電容量值，無法滿足更高之需求，發展下一世代高能量密度、高安全性、低成本、長壽命之儲能裝置乃是刻不容緩。針對此議題，可充放電之不同金屬電池因具有下列優點而非常具有潛力：(1) 使用低還原電位金屬實現更高能量密度 (如鋰金屬)；(2) 可與轉化型正極材料(如硫、氧氣)搭配得到更高電容量與能量密度；(3)可透過組裝無陽極金屬電池進一步提升能量密度，且大幅降低生產成本與增加安全性；(4)使用地球富含與化學更加穩定之金屬元素(如鋅、鋁)作為負極材料以大幅降低生產成本與提升安全性。然而，如何提升金屬電池之充放電效能以達成商業化標準有賴於對正負極材料之反應機制的基礎科學了解，包括不同正極材料之充放電反應機制與金屬負極之沉積溶解機制。為此，臨場與原位之光譜與影像技術可做為一非常有力的工具用來分析材料結構與形貌在電池充放電過程中的演變，對於探索電化學儲能材料提供深入且全面的洞見。
本研究透過不同臨場(in-situ)與原位(in-operando)之光譜與影像技術探索不同金屬電池內部的各種反應機制，共分為三大主題與四個章節。第一章節旨在解析硫化聚丙烯腈(Sulfurized-polyacrylonitrile, S-cPAN)之分子結構與其合成機制，透過結合密度泛函理論計算(Density Function Theory, DFT)、X射線光電子能譜學與固態核磁共振光譜分析，提出S-cPAN分子結構中含有兩種氮原子環境(吡啶氮與吡咯氮)存在。此雙重氮環境不僅在材料合成時有效吸附S2分子，且催化了N-S共價鍵的生成，有別於以往文獻報導的單一C-S共價鍵。此外，透過理論計算之結果，本研究亦提出此兩種共價鍵於材料合成時的生成機制。
第二部分則利用臨場拉曼光譜與X光吸收光譜，結合DFT理論計算，解析S-cPAN在鋰硫電池中的充放電機制。結果顯示，有別於傳統硫碳復合正極之「固態-液態-固態」轉化反應，S-cPAN進行一「固態-固態」轉化反應。小分子硫(-Sx-, 2≤x≤4)透過C-S與N-S共價鍵附著於PAN之高分子鏈上，在放電池透過先斷開S-S共價鍵後斷開C-S與N-S共價鍵，直接於高分子鏈上還原，進而消除了多硫化物(Polysulfides)的穿梭效應(Shuttle-effect)。此外，亦發現碳化PAN之高分子鏈會參與其電荷補償反應，且可在S-cPAN完全鋰化時有效的化學性吸附硫化鋰(Li2S)於高分子鏈含氮側，進而提高此硫化高分子之反應可逆性與穩定性。
其次在第三部分結合臨場光學顯微鏡(Optical Microscopy, OM)與穿透視X光顯微鏡(Transmission X-ray Microscopy, TXM)技術觀測鋰金屬之沉積溶解行為，提出其對應之成核(Nucleation)、枝晶(Dendrite)/失活鋰(Dead-Li)生長機制。並提出一整合式解析策略(Integrated protocol)進行無陽極鋰金屬電池(Anode-free Li-metal batteries, AFLMBs)中之各項不可逆庫倫效率的來源判別與定量分析。透過分析此整合策略拆解出之訊息，能對無陽極鋰金屬電池乃至鋰金屬電池皆擁有更深入的了解，對於未來的研究提供更全面的認識與方向。
第四部分透過互補的原位X光繞射光譜與TXM觀測並探討鋅金屬於高濃度雙鹽類水系電解液中沉積溶解時之結構與形貌演化，以及與其相關之鈍化層(Passivation layer)生成機制。結果顯示高濃度鹽類可有效降低自由水分子(Free water)含量，抑制鋅金屬水解副反應的發生，並生成堅固且較為平滑的鈍化層以抑制枝晶生長。研究結果對於水系電解液設計與鋅枝晶抑制提出洞見的資訊。
本研究展示了臨場與原位之光譜影像技術在解析電化學能源材料內部的複雜反應機制，與金屬電池中不同金屬沉積溶解行為扮演的重要角色。透過臨場與原位技術得到之深入且全面的訊息，可對於近一步提升金屬電池充放電效能提出有效的策略，最終實現商業化高能量密度、高安全性、低成本且長循環壽命的電化學儲能裝置。

With the surging growth of energy demand from electric vehicles and portable electronics, the current lithium-ion battery technology approaches its theoretical limit regarding energy density and specific capacity. The development of next-generation energy-dense, high safety, and long lifespan battery technologies has never been more critical. In this regard, rechargeable metal batteries are promising solutions due to due to several reasons: (1) use of low reduction potential metal to realize higher energy density (e.g., Li, -3.04 V vs. SHE); (2) capable of pairing with conversion-type but metal-ion deficient cathodes with higher specific capacity (e.g., Li-S, Li-air batteries); (3) anode-free metal batteries to achieve even higher energy density with ease of fabrication and high safety; (4) the use of earth-abundant and chemically stable metals as anode material for low-cost and safe batteries (e.g., Zn and Al). However, the further improvement of each metal-based battery on their performance meeting the commercialization criteria still relies on the fundamental understanding of reaction mechanisms at both cathode and anode electrodes, including redox reactions of cathode materials and metallic anode deposition/stripping mechanisms. For this purpose, in-situ/operando imaging and spectroscopy techniques are powerful tools to probe the structural and morphological evolution of electrode materials, which could provide in-depth insights on exploring various electrochemical energy materials.
This dissertation describes the development of rechargeable metal-based batteries and the utilization of advanced imaging and spectroscopy techniques to unravel the underlying reaction mechanisms within them. The first part of this work identified the molecular structure of sulfurized-polyacrylonitrile (S-cPAN) through the combination of ex-situ X-ray Photoelectron Spectroscopy (XPS), solid-state nuclear magnetic resonance (ssNMR), and density functional theory (DFT). The coexistence of pyridinic/pyrrolic nitrogen (NPD/NPL) is observed and reported for the first time. This plays a vital role in attracting S2 molecules and facilitating N−S bond formation apart from the generally accepted C−S bond in S-cPAN. The new findings suggest a more reasonable S-cPAN molecular structure to address this longstanding debate.
In the second part of this work, using experimental in-situ Raman spectroscopy and X-ray absorption spectroscopy (XAS) and DFT calculation, lithiation/delithiation mechanism of S-cPAN in Li-S battery is studied. The results show a solid-solid transformation reaction during the lithiation/delithiation of S-cPAN, with the cPAN backbone involves in the charge compensation that chemically absorbs Li2S along the nitrogen edge of cPAN matrix. The proposed modified mechanism deciphers the outstanding electrochemical performance of S-cPAN, providing a new pathway for designing high capacity, shuttle-free cathode materials for next-generation Li–S batteries, and a new perspective of sulfur chemistry.
The third part of this work focuses on investigating Li deposition/stripping mechanism and determining the sources of irreversible Coulombic efficiency (irr-CE) anode-free Li-metal batteries (AFLMBs), respectively. In-situ optical microscopy (OM) and transmission X-ray microscopy (TXM) are employed to unravel the information of Li growth including nucleation process and dendrite/dead-Li formation. Furthermore, an integrated protocol combining different types of cell configuration is presented to determine various sources of irreversible coulombic efficiency in anode-free lithium metal cells. The decrypted information from the protocol provides an insightful understanding of the behaviors of LMBs and AFLMBs, which promotes their development for practical applications.
Lastly, with the complementary results obtained from in-operando X-ray diffraction and TXM, the structural and morphological evolution of Zn deposition/stripping with the relating passivation layer formation is comprehensively monitored and studied, providing insightful information of the Zn dendrite suppression and inhibiting electrolyte decomposition in aqueous Zn-metal batteries (AZMBs).
In general, this work demonstrates the critical role that in-situ/operando spectroscopy and imaging techniques play in understanding the intricate reaction mechanisms of electrochemical energy materials and the metal deposition/stripping behaviors. With the valuable and in-depth understanding gained from the in-situ/operando characterization techniques, practical strategies for further improving the cycle performance and lifespan of rechargeable metal-based batteries can be developed, leading to the realization of energy-dense, low-cost, and high safety energy storage systems with long-term stability.

摘要    I
ABSTRACT    III
ACKNOWLEDGEMENTS    V
SYMBOLS    XI
ABBREVIATIONS    XII
LIST OF FIGURES    XIV
LIST OF TABLES    XIX
Chapter 1    Introduction and Background    1
1    Electrochemical cells    2
2    Rechargeable metal batteries    3
3    Lithium-sulfur batteries    6
3.1    Fundamental principle and development roadmap    6
3.2    Carbonaceous composites    9
3.3    Metal oxides and metal sulfides    11
3.4    Lithium sulfide (Li2S)    12
3.5    Sulfurized-polymer and sulfurized polyacrylonitrile (S-cPAN)    12
4    Anode-free Lithium Metal Batteries    14
4.1    Fundamental principle and development roadmap    14
4.2    Surface engineering on current collector    17
4.3    Functional electrolytes    17
4.4    Electrolyte additives    18
4.5    Testing protocols    19
4.6    Electrode architecture    20
4.7    Fundamental studies    20
5    Aqueous Zinc-Metal Batteries    22
5.1    Fundamental principle and development roadmap    22
5.2    Early study on Zn dendrite growth    24
5.3    Functional Additives    24
5.4    Artificial surface coating    24
5.5    Electrolyte formulation    25
5.6    Modification of substrate    25
5.7    Anode-free ZMB    26
6    In-operando/situ spectroscopy and imaging techniques for battery researches    27
6.1    In-situ/operando spectroscopy techniques    27
6.2    In-situ/operando imaging techniques    32
7    Motivation and scope    37
7.1    Molecular structure and reaction mechanisms of S-cPAN    37
7.2    Dead-Li formation and irreversible reactions in AFLMBs    38
7.3    Zn deposition/stripping mechanism in aqueous electrolyte    38
Chapter 2    Experimental details and characterization techniques    39
1    Material preparation    39
1.1    Synthesis of S-cPAN    39
1.2    Synthesis of S-cPEG    39
1.3    Synthesis of S/C composites    39
1.4    Anode-free Li-metal battery    39
1.5    Cell assembly    40
2    XPS    41
2.1    Fundamental principle    41
2.2    Experimental considerations    41
3    Solid-state nuclear magnetic resonance spectroscopy    42
3.1    Magic-angle spinning (MAS)    43
3.2    ssNMR measurements    43
4    Raman spectroscopy    44
4.1    Fundamental principle    44
4.2    Experimental considerations    45
5    X-ray absorption spectroscopy    46
5.1    Fundamental principle    46
5.2    Experimental considerations    48
6    Optical microscopy    50
6.1    Experimental considerations    50
6.2    In-situ/operando OM measurements    50
7    Transmission X-ray microscopy    51
7.1    Experimental considerations    51
8    X-ray powder diffraction    52
8.1    Experimental considerations    53
8.2    In-operando XRD measurements    54
9    Electrochemical tests    55
9.1    Li-S batteries    55
9.2    Anode-free cells    56
Chapter 3    New Insights into the N-S Bond Formation of Sulfurized-Polyacrylonitrile Cathode Material for Lithium-Sulfur Batteries    57
1    Synopsis    57
2    Results and discussion    57
2.1    Electrochemical performance of S-cPAN vs. S-cPEG    57
2.2    Chemical environment of S-cPAN unraveled by spectroscopic techniques    59
2.3    Cooperation with DFT calculation    62
3    Summary    66
Chapter 4    Origin of Shuttle-Free Sulfurized Polyacrylonitrile in Lithium-Sulfur Batteries        67
1    Synopsis    67
2    Results and discussion    68
2.1    Characterization and Electrochemical Property    68
2.2    Computed Raman Spectra    73
2.3    In-situ Raman Measurement    75
2.4    XAS Analysis of S-cPAN    79
2.5    Solid-solid transformation mechanism of S-cPAN    82
3    Summary    86
Chapter 5    Decoupling the Origins of Irreversible Coulombic Efficiency in Anode-Free Lithium Metal Batteries    87
1    Synopsis    87
2    Results and discussion    88
2.1    In-situ OM observation of Li deposition/dissolution    88
2.2    Li nucleation and deposition/dissolution mechanism    89
2.3    Proposed integrated protocol    91
2.4    Procedures to obtain irr-CEs in different cell configurations    99
2.5    Experimental validation for the proposed protocol    101
2.6    Comparison of Initial Overpotential and Polarization at 50% SOC    103
2.7    Calculation of average coulombic efficiency of NMC//Li and NMC//Cu cells        103
2.8    Example 1: 1M LiPF6 in EC:DEC under 0.2 mA cm-2    104
2.9    Example 2: 1M LiPF6 in EC:DEC under 0.4 mA cm-2.    105
2.10    Example 3: 1M LiPF6 in EC:DEC with 5% FEC.    107
3    Summary    110
Chapter 6    In-operando Characterized Zn Deposition and Stripping behavior in aqueous electrolyte    111
1    Synopsis    111
2    Results and discussion    112
2.1    Morphological evaluation of Zn plating/stripping    112
2.2    Formation of passivation layer in Zn||Cu cell studied by in-operando XRD        118
2.3    Structural evolution of LFP cathode material in Zn||LFP cell    121
3    Summary    123
Chapter 7    Conclusion and perspective    125
1    Conclusion    125
2    Perspective    126
References    127

                                

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