全固态锂离子电池正极与石榴石型固体电解质界面的研究进展

doi:10.15541/jim20180512

无机材料学报 ›› 2019, Vol. 34 ›› Issue (7): 694-702.DOI: 10.15541/jim20180512

所属专题：离子电池材料

全固态锂离子电池正极与石榴石型固体电解质界面的研究进展

李栋^1,²,雷超^1,²,赖华³,刘小林^1,²,姚文俐^1,²,梁彤祥¹,钟盛文^1,²

^1. 材料科学与工程学院江西理工大学
^2. 江西省动力电池及材料重点实验室
^3. 资源环境与工程学院, 赣州341000

收稿日期:2018-10-31 修回日期:2019-01-15 出版日期:2019-07-20 网络出版日期:2019-06-26
作者简介:李栋(1982-), 男, 博士, 讲师. E-mail:libehave@jxust.edu.cn
基金资助:
国家自然科学基金(51874151);江西省教育厅一般项目(GJJ170510);江西省科技支撑计划项目(20151BBE50106)

Recent Advancements in Interface between Cathode and Garnet Solid Electrolyte for All Solid State Li-ion Batteries

LI Dong^1,²,LEI Chao^1,²,LAI Hua³,LIU Xiao-Lin^1,²,YAO Wen-Li^1,²,LIANG Tong-Xiang¹,ZHONG Sheng-Wen^1,²

^1. School of Materials Science and Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, China
^2. Jiangxi Key Laboratory of Power Battery and Materials, Jiangxi University of Science and Technology, Ganzhou 341000, China
^3. School of Resources and Environmental Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, China

Received:2018-10-31 Revised:2019-01-15 Published:2019-07-20 Online:2019-06-26
Supported by:
National Natural Science Foundation of China(51874151);General Program by Jiangxi Provincial Department of Education(GJJ170510);Science and Technology Support Project of Jiangxi Province(20151BBE50106)

摘要/Abstract

摘要：

全固态锂离子电池具有高安全性、高能量密度、宽使用温度范围以及长使用寿命等优势, 在动力电池汽车和大规模储能电网领域具有广阔的应用前景。作为全固态电池的重要组成部分, 无机固体电解质尤其是石榴石型固态电解质在室温下锂离子电导率可达10 ^-3 S·cm ^-1, 且对金属锂相对稳定, 在全固态电池的应用中具有明显的优势。然而正极与石榴石型固体电解质间接触性能以及界面的稳定性差, 使得电池表现出高的界面阻抗、低的库伦效率和差的循环性能。本文以全固态锂离子电池正极与石榴石型固体电解质界面为研究对象, 分析了正极/固体电解质的界面特性以及界面研究中存在的问题, 综述了正极复合、界面处理工艺、界面层引入等界面调控和改性的方法, 阐述了优化正极与石榴石型固体电解质界面结构, 改善界面润湿性的解决思路, 提出了未来全固态锂离子电池发展中有待进一步改进的关键问题, 为探索全固态锂离子电池的实际应用提供了借鉴。

关键词: 无机固体电解质, 复合电解质, 界面润湿性, 界面阻抗, 界面改性, 综述

Abstract:

All-solid-state lithium battery (ASSLB) with inorganic solid state electrolytes is one of promising candidates for electric vehicles and large-scale smart grids for storage of alternative energy resources due to their benefits in safety, energy density, operable temperature range, and longer cycle life. As the key component in ASSLB, inorganic lithium-ion-based solid-state electrolytes (SSEs), especially the garnet-type solid electrolytes that own ionic conductivities in the order of 10 ^-3 S·cm ^-1 at room temperature and are relative safe vs. Li metal, have obvious advantages in ASSLB. However, interfacial instability and their poor solid-solid contact between garnet and cathode result in high interfacial resistance, low efficiency, and poor cycle performance. Based on these understandings and analyses of interface characteristics and issues, this work presents a brief review on modification of interface, covering composite cathode, composite electrolyte, interface engineering, and interface layer．Some approaches of improving interface wettability and future research directions of ASSLB are given as well, which endeavor to realize the practical applications of ASSLB.

Key words: inorganic solid state electrolyte, composite electrolyte, interfacial wettability, interfacial impendence, interface modification, review

中图分类号:

TM911

李栋, 雷超, 赖华, 刘小林, 姚文俐, 梁彤祥, 钟盛文. 全固态锂离子电池正极与石榴石型固体电解质界面的研究进展[J]. 无机材料学报, 2019, 34(7): 694-702.

LI Dong, LEI Chao, LAI Hua, LIU Xiao-Lin, YAO Wen-Li, LIANG Tong-Xiang, ZHONG Sheng-Wen. Recent Advancements in Interface between Cathode and Garnet Solid Electrolyte for All Solid State Li-ion Batteries[J]. Journal of Inorganic Materials, 2019, 34(7): 694-702.

图/表 8

图1 室温下不同类型固体电解质的电导率[17]

Fig. 1 Conductivity of different types of solid electrolytes at room temperature[17]

图2 0到5 V(vs. Li), 电解质/正极界面相形成能[蓝色, LCO; 红色, LMO; 绿色, LFP; 粗线, LLZO; 细线, LLTO], 计算得到的材料内在稳定窗口如图中底部行线所示[50]

Fig. 2 Driving force for interphase formation between electrolyte, and cathode, with varying voltage from 0 to 5 V vs lithium metal [Legend: blue, LCO; red, LMO; green, LFP; thick line, LLZO; thin line, LLTO]. The calculated intrinsic stability windows are marked along the bottom for reference[50]

图3 (a)复合阴极/LLZTO电解质界面的SEM照片; (b) LLZTO电解质表面的SEM照片; 在(c)二次电子和(d)背散射电子下的复合阴极的SEM照片[53]

Fig. 3 (a) Typical scanning electron microscope (SEM) image of the interface between composite cathodes and LLZTO electrolyte; (b) SEM image for the surface of LLZTO ceramic; SEM images of the composite cathodes which were measured in (c) the second-electron and (d) the back-scatter-electron mode[53]

图4 ASSLB的合成过程示意图[57]

Fig. 4 Schematic illustration of the synthesis procedure[57] (a) Microscale LLZO particles; (b) Nanoscale LLZO particles; (c) Nanoscale LLZO slurry; (d) Cathode layer of LFP; (e) LLZO film; (f) All-solid-state battery of Li/LLZO/LFP

图5 (a)界面引入Nb层改性前后的LLZO/LiCoO2界面示意图; (b) Nb层改性后LLZO/LiCoO2界面的截面-HAADF-STEM照片, 虚框为元素分布图[65]

Fig. 5 (a) Schematic illustrations of non-modified and Nb-modified LLZ/LiCoO2 interfaces. The mutual diffusion between LLZO and LiCoO2 produces non-Li+-conductive phases such as a crystalline La2CoO4 phase. Nb-modified LLZ/LiCoO2 interface suppresses the mutual diffusion and produce Li+-conductive amorphous phase; (b) Cross-sectional-HAADF-STEM image of a Nb-modified interface between LLZO and LiCoO2[65]. EDX elemental mappings in (b) for Co (red), Nb (purple), and La (green) are overlaid in the dashed-line-enclosed region. The top Pt is a protective layer for FIB processes

图6 含15wt%聚合物的LFP复合阴极与LLZTO复合电解质的界面SEM照片[72]

Fig. 6 SEM image of the interface between LFP composite cathode containing 15wt% polymer and the LLZTO composite electrolyte[72]

图7 PEO/LLZTO@IL膜合成和全固态电池示意图[78]

Fig. 7 Solid-state LFP or LFMP/Li cells using PEO/LLZTO@IL membranes[78]

表1 以Li7La3Zr2O12石榴石型固体电解质组装的全固态电池性能

Table 1 Performances of ASSLBs based on garnet-type Li7La3Zr2O12 solid electrolytes

Electrolyte	Ion-conductivity/ (mS·cm^-1)	Cathode materials	Interface Engineering	Test condition	Discharge capacity /(mAh·g^-1)	Ref.
Li_6.20Ga_0.30La_2.95Rb_0.05Zr₂O₁₂	1.62	LiFePO₄	Coating	60 ℃, 5 μA·cm^-2 2.8-4.0 V	152(1^st), 110(20^th)	[24]
Li_6.4La₃Zr_1.4Ta_0.6O₁₂	1.60	LiFePO₄	Coating	60 ℃, 0.05C 2.76-4.00 V	150(1^st), 140(100^th)	[53]
Li₇La₃Zr₂O₁₂	2.40	LiFePO₄	Coating	25 ℃ 0.1C	160.4 (1^st), 136.8 (100^th)	[57]
Li_6.75La₃Zr_1.75Nb_0.25O₁₂	1.67	LiCoO₂	PLD	25 ℃, 3.5 μA·cm^-2 2.5-4.2 V	129 (1^st), 127(100^th)	[61]
Li_6.8(La_2.95Ca_0.05)(Zr_1.75Nb_0.25)O₁₂	0.36	LiCoO₂	Co-sintering	1 μA·g^-1, 3.0-4.2 V	78(1^st)	[47]
Li₇La₃Zr₂O₁₂(1.7wt% Al, 0.1wt% Si)	0.68	LiCoO₂	PLD	1 mA·cm^-2, 3.2-4.2 V	80 (1^st)	[65]
Li_6.75La₃Zr_1.75Nb_0.25O₁₂	1.23	LiCoO₂	Screen-printing	25 ℃, 10 μA·cm^-23.00-4.05 V	85(1^st)	[64]
Li_6.75La₃Zr_1.75Ta_0.25O₁₂	～1.00	LiCoO₂	Coating+ co-sintering	5 μA·cm^-2	101.3(1^st)	[54]
Li_6.75La₃Zr_1.75Ta_0.25O₁₂	0.74	LiNi_0.5Co_0.2Mn_0.3O₂	Tape casting	80 ℃, 5 μA·cm^-23.0-4.6 V	123.3 (1^st), 76.6 (5^th)	[56]
Li_6.25Al_0.25La₃Zr₂O₁₂	0.50	Li₄Ti₅O₁₂	Coating	95 ℃, 2-8 μA·g^-1 1.0-2.5 V	15(1^st)	[81]

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全固态锂离子电池正极与石榴石型固体电解质界面的研究进展

Recent Advancements in Interface between Cathode and Garnet Solid Electrolyte for All Solid State Li-ion Batteries

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