Research progress of PEO-based composite solid-state electrolytes for lithium batteries
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摘要: 固态锂离子电池能量密度高、安全性强，是突破电池技术瓶颈的关键，受到了学术界和工业界的广泛关注。固态电解质是固态电池的核心，其中聚氧化乙烯(PEO)基聚合物固态电解质在改善电极界面相容性方面具有优势，是最有潜力的电解质材料之一。本文系统阐述了PEO与无机填料间的协同作用，及其对复合固态电解质的离子传输性和界面相容性的影响机制。首先对PEO基复合固态电解质做出概述，并探讨离子传输相关机制，然后分别综述了PEO-惰性填料和PEO-活性填料复合固态电解质体系的设计、制备、性能及机制，最后，对复合固态聚合物电解质的未来发展和优化设计做出展望。
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关键词:
- 固态锂电池 /
- 聚氧化乙烯 /
- 复合固态聚合物电解质 /
- 离子传输机制 /
- 无机填料
Abstract: Featured with high energy density and sound safety, solid-state lithium-ion battery is the key to breaking through the bottleneck shackling battery technology, gathering wide attention from academia and industry. Solid-state electrolytes are the core of solid-state batteries, among which polyethylene oxide (PEO) polymer solid-state electrolyte excels at improving electrode interface compatibility and is one of the most potential electrolyte materials. This paper systematically elucidated the synergistic effect of PEO with inorganic modified fillers and its influence on ion transport and interfacial compatibility of composite solid-state electrolytes. Following an overview of the PEO-based composite solid-state electrolyte, the mechanism of ion transport was discussed. Then, the design, preparation, performance, and mechanism of PEO-inert filler and PEO-active filler composite solid-state electrolyte systems were reviewed respectively. Finally, an outlook on the future development and optimization design of composite solid-state polymer electrolytes was presented. -
图 3 (a) Li+分别在PEO相中、PEO相和PEO/陶瓷界面处、PEO相和陶瓷相以及PEO/陶瓷界面处的传导途径示意图[45]；(b) 锂离子在LLZO (5wt%) -PEO (LiTFSI)、LLZO (20wt%) -PEO (LiTFSI) 和LLZO (50wt%) -PEO (LiTFSI)复合电解质中的路径示意图[46]；(c) NPs、无序NWs和排列NWs在复合聚合物电解质中的锂离子传导途径[48]；(d) 填料、聚合物和锂盐之间的路易斯酸碱相互作用示意图[36]
Figure 3. (a) Schematic illustration of the Li+ conduction pathways in the PEO phase,PEO phase and PEO/ceramic interface,PEO phase and ceramic phase and PEO/ceramic interface, respectively[45]; (b) Schematic of Li-ion pathways within LLZO (5wt%)–PEO (LiTFSI), LLZO (20wt%)–PEO (LiTFSI) and LLZO (50wt%)–PEO (LiTFSI) composite electrolytes[46]; (c) Li-ion conduction pathways in composite polymer electrolytes with NPs,random NWs and aligned NWs[48]; (d) Illustration of Lewis acid-base interaction between fillers, polymer, and Li salt[36]
图 4 (a) 三种不同类型Al2O3与PEO的表面相互作用和Al2O3-PEO CSPEs的电导率图[56]；(b) AAO -聚合物复合电解质制备工艺示意图[58]；(c) 分别为AAO圆盘中单个纳米通道中聚合物电解质示意图、各组分的离子电导率、界面离子电导率以及AAO-聚合物复合电解质(APCE)界面层厚度[58]；(d) 功能化Al2O3 (F- Al2O3)的合成及其制备杂化聚合物电解质(HPE)[59]；分散在硅片上PEO薄膜中的颗粒的SEM图像: (e) Al2O3, ( f) F- Al2O3[59]
Figure 4. (a) Surface interactions between three diferent type Al2O3 and PEO and conductivity plots of Al2O3-PEO CSPEs[56]; (b) Schematics of fabrication procedures of AAO-polymer composite electrolyte[58]; (c) Schematics of polymer electrolyte in individual nanochannel of the AAO disc, the ionic conductivities of each component, the interface ion conductivities, and the thickness of interfacial layer of AAO-polymer composite electrolyte (APCE), respectively[58]; (d) Synthesis of functionalized Al2O3 (F-Al2O3) and preparation of hybrid polymer electrolyte (HPE) using F-Al2O3[59]; SEM images of the particles dispersed in PEO film on a Si wafer: (e) Al2O3, (f) F- Al2O3[59]
图 5 (a) PEO链与MUSiO2的原位水解过程及相互作用机制示意图[60]；(b) SiO2-Li2SO4-PEO CSPEs的制备工艺示意图以及由Li2SO4衍生的SiO2纤维CSPE实现Li+快速传导的原理图[61]；(c) 原位水解制备CSPEs的示意图[62]；(d) 不同成分聚合物电解质的离子电导率[65]；(e) PEO-LiTFSI电解质和PEO-LiTFSI -3 wt% TiO2@PDA复合电解质的DSC曲线[65]；(f) CPEs中缺氧TiO2表面相互作用示意图[66]；TiO2样品的XPS光谱(g)和Ti 2 p的高分辨率光谱(h)[67]
Figure 5. (a) Schematic figures showing the procedure of in situ hydrolysis and interaction mechanisms among PEO chains and MUSiO2[60]; (b) Schematic diagram of preparation process of SiO2/Li2SO4/PEO CSPEs and schematics of fast Li+ conduction enabled by the Li2SO4-derived SiO2 fibers CSPEs [61];(c) The schematic diagram of CPSEs prepared by in situ hydrolysis[62]; (d) The ionic conductivities of the polymer electrolytes with different compositions[65]; (e) DSC curves of the PEO–LiTFSI electrolyte and PEO–LiTFSI-3 wt% TiO2@PDA composite electrolyte[65]; (f) Schematic illustrations of surface interaction of oxygen-deficient TiO2 in CPEs[66]; XPS survey spectra of the TiO2 sample (g) and high-resolution spectra of the Ti 2 p (h)[67]
图 6 (a) 锂对称电池中多尺度排列的介孔石榴石Li6.4La3Zr2Al0.2O12 (LLZO)膜与聚合物电解质结合示意图[81]；(b) 石榴石-木膜阻抗随温度升高而下降的Nyquist图，插图为测试单元的结构[81]；(c) 石榴石木和PEO聚合物电解质在不同温度下的离子电导率对比示意图[81]；(d) 以陶瓷石榴石纳米纤维为增强层，锂离子导电聚合物为基体的复合固态电解质示意图[83]；(e) 纤维素衍生的CPE的制备工艺示意图[88]；(f) 纤维素/陶瓷增强CPE中Li+导电机制示意图[88]；(g) PEO|PEO−钙钛矿|PEO复合电解质的表面SEM图像、横截面SEM图像及横截面形貌详细视图[90]
Figure 6. (a) Schematic of multi-scale aligned mesoporous garnet Li6.4La3Zr2Al0.2O12 (LLZO) membrane incorporated with polymer electrolyte in a lithium symmetric cell[81]; (b) Nyquist plot showing the decrease in the impedance of the garnet-wood membrane with increasing temperature, the inset schematic shows the structure of the testing cell[81]; (c) Comparison of the ionic conductivity of the garnet-wood and PEO based polymer electrolyte at different temperatures[81]; (d) Schematic of the composite solid electrolyte, where ceramic garnet nanofibers function as the reinforcement and lithium-ion conducting polymer functions as the matrix[83]; (e) Schematic illustration of fabrication procedures for the cellulose derived CPE[88]; (f) Schematic of proposed Li+ conducting mechanism in the cellulose/ceramic reinforced CPE[88]; (g) SEM image of the surface, cross-sectional SEM image and detailed view of the cross-section morphology of the PEO|PEO−perovskite|PEO composite electrolyte[90]
表 1 PEO基复合固态电解质文献报道汇总
Table 1. Summary of literature reports on PEO-based composite solid electrolyte
Polymer matrix lithium salt Filler Ionic Conductivity/( S·cm−1) ESW/(V vs.Li/Li+) tLi+ Ref. PEO LiTFSI Al2O3 5.82 ×10−4 (RT) — — [58] PEO LiTFSI Al2O3 9.6 ×10–4 (25℃) 5 0.81 [97] PEO LiTFSI SiO2 1.8 ×10–4 (30℃) 5.3 0.42 [62] PEO LiClO4 SiO2 1.2 ×10–3 (60℃) >5.5 — [98] PEO LiClO4 SiO2 1.1 ×10–4 (30℃) >4.8 — [99] PEO LiClO4 TiO2 1 ×10–5 (30°C) 5 0.3 [100] PEO LiTFSI TiO2@PDA 4.36 ×10–4 (55°C) 5 0.19 [65] PEO LiTFSI Ti3+-TiO2 1 ×10–4 (30℃) 5.5 0.36 [67] PEO LiBF4 ZrO2 4.4 ×10–4 (80℃) — 0.68 [72] PEO LiCF3SO3 ZrO2 1.38 ×10–4 (RT) — — [74] PEO LiTFSI LLZTO 1.9 ×10–4 (40℃) 5.1 0.67 [101] PEO LiTFSI LLZTO 3.03×10–4 (55℃) 4.5 0.117 [102] PEO LiTFSI LLZTO 5.6×10–4 (60℃) 4.75 0.46 [103] PEO LiTFSI LLZO 5.5×10–4 (30℃) >5.7 0.21 [104] PEO LiTFSI LLZO 2.39 ×10–4 (25℃) >5.5 — [105] PEO LiTFSI LATP 4 ×10–4 (60℃) 4.7 — [106] PEO LiTFSI LATP 3.61×10–4 (60℃) 4.8 — [107] PEO LiTFSI LAGP 6.76×10–4 (60℃) 5.3 0.378 [108] PEO LiTFSI LAGP 1.6×10–5 (20℃) — — [109] PEO LiTFSI LLTO 2.04×10–4 (25℃) 4.7 — [110] PEO LiTFSI LLTO 2.3×10–4 (RT) 4.5 — [111] PEO LiTFSI LLTO 1.8×10–4 (RT) 4.5 0.33 [112] PEO LiTFSI LGPS 1.21×10–3 (80℃) 5.7 0.26 [95] PEG-PEO LiTFSI LGPS 9.83×10–4 (RT) — 0.68 [96] Notes: ESW is Electrochemical stability window; tLi+ is Lithium-ion transference number; RT is Room Temperature; PDA is polydopamine; LLZTO is Li6.4La3Zr1.4Ta0.6O12/Li6.75La3Zr1.75Ta0.25O12; LLZO is Li7La3Zr2O12; LATP is Li1.4Al0.4Ti1.6(PO4)3; LAGP is Li1.5Al0.5Ge1.5(PO4)3; LLTO is Li0.33La0.557TiO3; LGPS is Li10GeP2S12; PEG is Polyethylene glycol. 
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