水熱法合成之Li1+xAlxTi2-x(PO4)3與聚偏二氟乙烯/醋酸纖維素複合型固態電解質 應用於鋰離子電池之研究

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趙思齊(Szu-Chi Chao) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

水熱法合成之Li1+xAlxTi2-x(PO4)3與聚偏二氟乙烯/醋酸纖維素複合型固態電解質應用於鋰離子電池之研究
(Study of Hydrothermally-Synthesized Li1+xAlxTi2-x(PO4)3 and Poly (vinylidenedifluoride)/Cellulose Acetate Composite Solid Electrolyte for Lithium-Ion Batteries)

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至系統瀏覽論文 (2027-6-30以後開放)

摘要(中)

本研究使用醋酸纖維素(Cellulose Acetate)及雙（三氟甲基磺醯）氨基鋰（Lithium bis(trifluoromethanesulfonyl)imide, LiTFSI）混摻於聚偏二氟乙烯（Poly(vinylidene) difluoride, PVDF）高分子中，接著添加水熱法合成之Li1.3Al0.3Ti1.7(PO4)3 （LATP）陶瓷粉末形成複合型固態電解質薄膜，並且更換不同的混摻物/PVDF高分子之比例、透過溶液澆鑄法開發具有最佳性能的複合型固態電解質薄膜。由結果可以得知此種複合型固態電解質薄膜具有寬廣的電位窗（~5 V）、高溫下的熱穩定性（~250 ℃）、以及機械可撓性，而將電解質薄膜配合少量電解液 (1 M LiTFSI in TEGDME) 應用於磷酸鐵鋰（LiFePO4, LFP）正極後，也表現出優異的電化學性能。在混摻適量的CA及LiTFSI至PVDF（PVDF: CA: LiTFSI = 4: 1: 4）後，其導電率可達到3.3⨉10-4 S cm-1，而放電容量則為139.8 mAh g-1 @ 0.1 C且維持穩定的庫倫效率（~100 %）。接著，為了進一步改善熱穩定性及電化學性能，使此電解質薄膜能應用在更多極端條件，在下一階段的研究中添加不同比例條件的LATP粉末至PVDF/CA/LiTFSI高分子電解質薄膜中，可發現當LATP陶瓷粉末添加量為20 wt%時具有最佳的電化學性能。在此摻雜比例下（PVDF: CA: LiTFSI: LATP = 4: 1: 4: 2），複合型固態電解質薄膜擁有6.6⨉10-4 S cm-1的導電率，而放電容量則被提升至162.1 mAh g-1 @ 0.1 C，並保有穩定的庫倫效率（~100 %）。此研究所開發的複合型固態電解質薄膜展現出優秀的電化學穩定性、高溫下的熱穩定性、高離子導電率及放電容量，同時採用了相對具有環境友善性的材料與製程，表明其應用於鋰離子電池的潛力。

摘要(英)

In this study, cellulose acetate (CA) and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) were added to poly(vinylidene) difluoride (PVDF) polymer, followed by the addition of hydrothermally-synthesized Li1.3Al0.3Ti1.7(PO4)3 (LATP) ceramic powder to form the composite solid electrolyte (CSE) membranes via solution casting method. Different dopant/PVDF ratios were investigated to develop a composite with optimal performance. From the results, it could be known that this CSE membrane had a wide potential window (~5 V), thermal stability at high temperatures (~250 °C), and mechanical foldability. The membranes showed excellent electrochemical performance after applying to LiFePO4 (LFP) cathode with a trace amount of liquid electrolyte (1 M LiTFSI in TEGDME). After mixing an appropriate amount of CA and LiTFSI into PVDF (PVDF: CA: LiTFSI = 4: 1: 4), the conductivity could reach 3.3⨉10-4 S cm-1, and the discharge capacity was 139.8 mAh g-1 @ 0.1 C and maintained stable Coulombic efficiency (~100 %). Then, to further improve the thermal stability and electrochemical performance enabled the electrolyte membrane to be used in more extreme environments, LATP powders in different weight ratios were added to the PVDF/CA/LiTFSI solid polymer electrolyte (SPE) membrane. Upon 20 wt% doping ratio (PVDF: CA: LiTFSI: LATP = 4: 1: 4: 2), the CPE membrane had a conductivity of 6.6⨉10-4 S cm-1, and the discharge capacity was enhanced to 162.1 mAh g-1 @ 0.1 C with stable Coulombic efficiency (~100 %). The CPE membrane developed in this research exhibited excellent electrochemical stability, thermal stability at high temperatures, and high ionic conductivity and discharge capacity. Also, the process and materials were relatively environmental-friendly, indicating its potential for applying for lithium-ion batteries (LIBs).

關鍵字(中)

★ 鋰離子電池
★ 固態電解質
★ 磷酸鈦鋁鋰
★ 醋酸纖維素
★ 環境友善

關鍵字(英)

★ Lithium-ion battery
★ Solid-state electrolyte
★ LATP
★ Cellulose acetate
★ Environmental-friendly

論文目次

摘要 i
Abstract iii
Acknowledgement v
Table of contents viii
List of figures xi
List of tables xvi
Chapter 1 Introduction 1
Chapter 2 Background 4
2-1 The lithium-ion batteries application and future development 4
2-1-1 Portable devices 4
2-1-2 Electric vehicles 5
2-1-3 Stationary energy storage systems 6
2-2 The basic concepts of lithium-ion batteries 6
2-3 The components of lithium-ion batteries 8
2-3-1 Cathode material 8
2-3-2 Anode material 9
2-3-3 Separator 10
2-3-4 Electrolyte 12
2-4 Solid state electrolyte 14
2-4-1 Inorganic solid-state electrolyte 15
2-4-2 LATP solid-state electrolyte synthesis 24
2-4-3 Development and challenge of LATP solid-state electrolyte 31
2-5 Polymer solid state electrolyte 33
2-5-1 PVDF-based polymer solid state electrolyte 35
2-6 Composite solid-state electrolyte 38
Chapter 3 Experiment 41
3-1 Experimental frame 41
3-2 Experimental chemicals and instruments 43
3-3 Experimental procedure 45
3-3-1 Preparation of Li1+xAlxTi2-x(PO4)3 solid electrolyte powder 45
3-3-2 Preparation of cellulose acetate / PVDF hybrid polymer 46
3-3-3 Preparation of LiTFSI-doped polymer solid electrolyte membrane 46
3-3-4 Preparation of LATP composite electrolyte membrane 47
3-3-5 Coin cell assembly and test 48
3-4 Materials analysis and electrochemical characterization 49
3-4-1 X-ray Diffraction (XRD) 50
3-4-2 Field Emission-Scanning Electron Microscopy (FE-SEM) 51
3-4-3 Thermogravimetric Analysis (TGA) 51
3-4-4 Differential Scanning Calorimetry (DSC) 52
3-4-5 Linear Sweep Voltammetry (LSV) 52
3-4-6 Electrochemical Impedance Spectroscopy (EIS) 53
Chapter 4 Result and discussion 54
4-1 Li1+xAlxTi2-x(PO4)3 inorganic electrolyte fabrication 54
4-1-1 X-ray diffraction-solvent composition effect 54
4-1-2 Surface morphology-precursor crystalline 57
4-1-3 X-ray diffraction-calcination temperature 59
4-1-4 Surface morphology-resulting LATP powder 61
4-2 PVDF/CA hybrid polymer fabrication 64
4-2-1 X-ray diffraction-hybrid polymer 64
4-2-2 Crystallinity analysis-hybrid polymer 66
4-2-3 Thermal stability-hybrid polymer 68
4-2-4 Surface morphology-hybrid polymer 70
4-2-5 Electrochemical stability-hybrid polymer 72
4-2-6 Electrochemical impedance spectroscopy-hybrid polymer 74
4-3 LiTFSI/CA/PVDF solid polymer electrolyte fabrication 76
4-3-1 X-ray diffraction 76
4-3-2 Crystallinity analysis-solid polymer electrolyte 78
4-3-3 Thermal stability-solid polymer electrolyte 80
4-3-4 Surface morphology-solid polymer electrolyte 82
4-3-5 Electrochemical stability-solid polymer electrolyte 88
4-3-6 Electrochemical impedance spectroscopy-solid polymer electrolyte 89
4-4 LATP/LiTFSI/CA/PVDF composite solid electrolyte fabrication 91
4-4-1 X-ray diffraction-composite solid electrolyte 91
4-4-2 Crystallinity analysis-composite solid electrolyte 93
4-4-3 Thermal stability-composite solid electrolyte 95
4-4-4 Surface morphology-composite solid electrolyte 97
4-4-5 Electrochemical stability-composite solid electrolyte 103
4-4-6 Electrochemical impedance spectroscopy-composite solid electrolyte 104
4-4-7 Charge and discharge test 107
4-4-8 Cycle Performance 109
Chapter 5 Conclusion and Prospect 111
5-1 Conclusion 111
5-1-1 Li1+xAlxTi2-x(PO4)3 inorganic electrolyte fabrication 111
5-1-2 LATP/LiTFSI/CA/PVDF composite solid electrolyte fabrication 112
5-2 Prospect 114
Chapter 6 Reference 115
2021 TWIChE poster I
2022 pre-oral poster II

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指導教授

劉奕宏

審核日期

2022-8-3

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