固态锂电池电极过程的原位研究进展

doi:10.6023/A21060255

化学学报 ›› 2021, Vol. 79 ›› Issue (10): 1197-1213.DOI: 10.6023/A21060255 上一篇下一篇

综述

固态锂电池电极过程的原位研究进展

田建鑫^a^,^b, 郭慧娟^a^,^b, 万静^a^,^b, 刘桂贤^a^,^b, 严会娟^a^,^b, 文锐^a^,^b^,^*(), 万立骏^a^,^b

a 中国科学院化学研究所中国科学院分子纳米结构与纳米技术重点实验室中国科学院分子科学科教融合卓越中心北京分子科学国家研究中心北京 100190
b 中国科学院大学北京 100049

投稿日期:2021-06-07 发布日期:2021-08-27
通讯作者: 文锐

作者简介:

田建鑫, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室2019级硕士研究生, 主要从事固态锂电池正极过程的原位研究.

郭慧娟, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室2018级博士研究生, 主要从事固态锂电池正极过程的原位研究.

万静, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室2017级博士研究生, 主要从事固态锂电池负极过程的原位研究.

刘桂贤, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室2018级博士研究生, 主要从事固态Li-S电池负极过程的原位研究.

严会娟, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室副研究员, 研究方向为扫描探针显微技术及应用.

文锐, 中国科学院化学研究所分子纳米结构与纳米技术重点实验室研究员、博士生导师, 国家自然科学基金优秀青年科学基金获得者, 主要研究领域是界面电化学.

万立骏, 中国科学院院士, 发展中国家科学院院士, 中国科学院化学研究所研究员、博士生导师, 国家杰出青年科学基金获得者, 主要从事扫描探针显微学、电化学和纳米材料科学的研究.

基金资助:
国家重点研发计划(2016YFA0202500); 国家自然科学基金优秀青年科学基金(21722508)

In Situ/Operando Advances of Electrode Processes in Solid-state Lithium Batteries

Jianxin Tian^a^,^b, Huijuan Guo^a^,^b, Jing Wan^a^,^b, Guixian Liu^a^,^b, Huijuan Yan^a^,^b, Rui Wen^a^,^b(), Lijun Wan^a^,^b

a Institute of Chemistry Chinese Academy of Sciences, CAS Key Laboratory of Molecular Nanostructure and Nanotechnology, CAS Research/Education Center for Excellence in Molecular Sciences, Beijing National Laboratory for Molecular Sciences, Beijing 100190, China
b University of Chinese Academy of Sciences, Beijing 100049, China

Received:2021-06-07 Published:2021-08-27
Contact: Rui Wen
Supported by:
National Key R&D Program of China(2016YFA0202500); National Natural Science Fund for Excellent Young Scholars(21722508)

文章分享

摘要/Abstract

固态锂电池(SSLBs)由于其安全性和潜在的高能量密度优势, 被认为是下一代动力电池的重要发展方向. 然而, 目前仍存在固态电解质离子电导率低, 电极/电解质界面兼容性和稳定性差等瓶颈问题. 为了提高SSLBs的性能, 阐明循环过程中电极、固态电解质及其界面间的动态演化是至关重要的. 在过去的几十年里, 各种先进原位表征技术的出现, 促进了对高性能锂电池内部工作机制的理解, 推动了SSLBs进一步发展. 本综述系统地介绍了近几年原子力显微镜、电子显微镜、X射线显微镜等成像表征技术和拉曼光谱、X-ray基技术、中子深度分析等成分分析技术的原位研究进展. 重点分析了各类表征技术在SSLBs循环过程中形貌和组分的演化, 包括正极材料的相变、形变, 金属锂的沉积/溶解、锂枝晶生长, 固态电解质结构演化和固体电解质中间相的形成, 进一步加深了对固态锂电池的理解.

关键词: 固态锂电池, 电极过程, 固体电解质中间相, 原位技术

Solid-state lithium batteries (SSLBs) are considered to be an important development direction for the next generation of power batteries due to their safety and potentially high energy density. However, there are several challenges including low ionic conductivity, poor stability/incompatibility between electrodes and electrolytes at present. To improve the performance of SSLBs, it is very important to clarify the dynamic evolution of electrodes, solid electrolytes, and their interfaces in the cycle process. In the past few decades, the emergence of various advanced in-situ characterization technologies has improved the understanding of the working mechanism of high-performance lithium batteries and promoted further development. Herein, we present a comprehensive overview of the in situ research progress of atomic force microscope, electron microscope, X-ray microscope and other imaging characterization techniques, and component analysis techniques such as Raman spectroscopy, X-ray technology, and neutron depth analysis in recent years. The focus is on the application research of various characterization techniques in morphology and composition evolution processes of the SSLBs, including the phase transformation and deformation of the cathode materials, the deposition/dissolution of lithium metal, the growth of lithium dendrites, the structure evolution of solid electrolytes, and the formation of the solid electrolyte interphase, which strengths the understanding of solid-state lithium batteries.

Key words: solid-state lithium battery, electrode process, solid electrolyte interphase, in situ technology

引用此文

田建鑫, 郭慧娟, 万静, 刘桂贤, 严会娟, 文锐, 万立骏. 固态锂电池电极过程的原位研究进展[J]. 化学学报, 2021, 79(10): 1197-1213.

Jianxin Tian, Huijuan Guo, Jing Wan, Guixian Liu, Huijuan Yan, Rui Wen, Lijun Wan. In Situ/Operando Advances of Electrode Processes in Solid-state Lithium Batteries[J]. Acta Chimica Sinica, 2021, 79(10): 1197-1213.

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图/表 14

图1. 固态锂电池电极过程的原位表征技术示意图

Figure 1. Schematic illustration of in situ characterization techniques of electrode processes in solid-state lithium batteries

	光学显微镜(OM)	扫描电子显微镜(SEM)	透射电子显微镜(TEM)	原子力显微镜(AFM)	X-ray computed tomo- graphy microscopy
探测源	可见光、激光等	电子束	电子束	探针	X-ray
样品操作环境	大气、真空及液相	真空	真空	大气、真空及液相	大气或真空
空间分辨率	200 nm	2 nm	0.1 nm	0.1 nm (Z)	50 nm
优势	时间分辨率高、对样品要求低	2~20万的放大倍数连续可调、景深大	同时获得样品形貌、晶体学和微观结构信息	对样品侵扰性小、 3D表面成像	无损3D成像
劣势	空间分辨率低	2D成像、不利于测量对电子束敏感的样品	制样复杂、不利于测量对电子束敏感的样品	受限于表面粗糙度、成像范围小	轻元素对比度较弱

表1. 成像技术比较

Table 1. Comparison of imaging techniques

图2. 原位TEM用于正极、负极和固体电解质中间相的研究. (a) 原位TEM装置[37]. (b) LiCoO2正极材料: 单晶-多晶转变、反相畴边界和相干孪晶界的形成[48]. (c) Li tip与LCO/SRO(SrRuO3)/STO(SrTiO3)(001)的反应[22]. (d) N-HPCSs球内锂电镀/剥离过程[52]. (e) 在1.0 V、1.2 V、1.4 V、1.6 V、2.0 V和2.2 V的电压下LCO/LPSCl界面的原位电荷密度分布[55]

Figure 2. In situ TEM studies for cathode, anode and solid eletrolyte interphase. (a) In situ TEM set-up. Reproduced with permission[37]. Copyright 2016, American Chemical Society. (b) Cathode materials of LiCoO2: the monocrystal-polycrystal transition, formation of antiphase domain boundaries and coherent twin boundaries. Reproduced with permission[48]. Copyright 2017, American Chemical Society. (c) The reaction between Li tip and LCO/SRO (SrRuO3)/STO(SrTiO3)(001). Reproduced with permission[22]. Copyright 2018, Wiley. (d) The Li plating/stripping cycle on a N-HPCS. Reproduced with permission[52]. Copyright 2020, Wiley. (e) In situ charge-density-distribution characterization of the LCO/LPSCl interface with bias voltages of 1.0 V, 1.2 V, 1.4 V, 1.6 V, 2.0 V and 2.2 V. Reproduced with permission[55]. Copyright 2020, Nature

图3. (a) AFM原理图. (b) 原位AFM电化学池

Figure 3. (a) Schematic of the basic principle of AFM. (b) In situ AFM electrochemical cell

	成像模式	探测的物理量
基本模式	轻敲模式AFM	悬臂振幅A
	接触模式AFM	悬臂弯曲度D
	扭转共振模式AFM	悬臂扭转量t
	峰值力AFM	探针-样品间的相互作用F
功能化模式	相位成像(Phase imaging)	悬臂振动相位φ
	横向力显微镜LFM	针尖-样品横向力L
	磁力显微镜MFM	悬臂振动相位φ或频率ω
	开尔文探针显微镜KPFM	样品表面电势V
	导电原子力显微镜C-AFM	针尖-样品间的电流
	扫描电化学显微镜SECM	样品电容随交变电压的变化率dC/dV

表2. 常见AFM成像模式

Table 2. Common imaging modes of AFM

图4. 原位AFM: (a) 复合电解质形貌图: a~e) 第一圈放电和f~h) 第一圈充电[68]. (b) 锂化过程中In电极上SEI壳层的演化. a) 循环伏安曲线. b~g, i~n, p) 不同电位下AFM图像和相应的DMT模量图. h, m) 电极表面高度剖面. o) 3D AFM皱折结构[69]. (c) NCM523电极表面CEI膜演化. a~g) 形貌和a'~g') DMT模量. h) 薄膜厚度的高斯统计分布直方图. i) 电极表面平均DMT模量[70]

Figure 4. In situ AFM images: (a) Topography images of SCEs: a-e) discharging and f-h) charging during the first cycle. Reproduced with permission[68]. Copyright 2020, Wiley. (b) Morphological evolution of the SEI shell on the In electrode upon lithiation/delithiation. a) Cyclic voltammogram curve. b-g, i-n, p) AFM images and corresponding DMT modulus mappings on the In electrode at different potentials. h, m) Height section profiles of the electrode surfaces. o) 3D AFM images of the wrinkle structures. Reproduced with permission[69]. Copyright 2021, American Chemical Society. (c) Evolution of CEI film on NCM523 electrode. a-g) Morphology and a′-g′) mapping of the DMT modulus. h) The gauss statistic distribution histograms of the film thickness. i) Average DMT modulus of the electrode surface. Reproduced with permission[70]. Copyright 2020, American Chemical Society

图5. 原位SEM形貌图: (a) 原位SEM装置图[72]. (b) 锂枝晶穿透LLZTO横截面的过程和流程图[27]. (c) Li-S电池中固态硫化物的演化过程[74]

Figure 5. In situ SEM topography images. (a) SEM experimental setup. Reproduced with permission[72]. Copyright 2018, American Chemical Society. (b) Cross-sectional morphology evolution of the lithium dendrite penetrates the LLZTO: topography images and schematic illustration. Reproduced with per- mission[27]. Copyright 2019, Elsevier. (c) Evolution of solid sulfur species in Li-S cell. Reproduced with permission[74]. Copyright 2016, Elsevier

图6. 原位OM成像. (a) 不同电位下的锂沉积/剥离[59]. (b) 充放电过程中固体电解质中间相演化[78]. (c) Ga-doped LLZO与Li接触后的机械应力演化[79]

Figure 6. In situ OM studies. (a) Li plating/stripping processes at different potentials. Reproduced with permission[59]. Copyright 2020, Wiley. (b) Evolution of the cathode electrolyte interphase. Reproduced with permission[78]. Copyright 2019, The Royal Society of Chemistry. (c) Mechanical stress of Ga-doped LLZO ceramic pellet contacting with Li foil. Reproduced with permission[79]. Copyright 2019, Elsevier

图7. 原位X-ray成像. (a) Li/LAGP/Li电池中LAGP的机械降解[82]: A)从3D断层扫描中提取的LAGP颗粒中心的二维切片. B) LAGP整体3D裂纹网状图. (b) 原位TXM-XANES成像[83]: 相位分布、FeS2锂化剖视图、FeS2和Fe的XANES光谱和相体积分数

Figure 7. In situ X-ray images. (a) Mechanical degradation of LAGP within a Li/LAGP/Li cell: A) 2D slices from the center of the LAGP pellet extracted from the 3D tomogram. B) 3D crack networks shown throughout the entire LAGP pellet. Reproduced with permission[82]. Cop- yright 2019, American Chemical Society. (b) Operando X-ray spectro- scopic nanotomography: phase distribution, cut-view of FeS2 at lithiated state, the XANES spectra of standard FeS2 and Fe and phase volume fraction obtained from 3D quantitative analysis. Reproduced with permis- sion[83]. Copyright 2019, Wiley

图8. 原位拉曼光谱. (a) Li-S电池: 硫化物的演化[68]. (b) h-BN包覆和未包覆的LLZTO[90]

Figure 8. In situ Raman spectra. (a) Li-S batteries: changes of sulfur species. Reproduced with permission[68]. Copyright 2020, Wiley. (b) The h-BN-coated LLZTO and uncoated LLZTO. Reproduced with permis- sion[90]. Copyright 2020, American Chemical Society

图9. 原位XPS: 充放电过程中Li 1s core level演化[101]

图10. 原位XANES对比循环过程中空白和包覆LNO的NCM811正极材料的S K-峰、Ni K-峰和充放电剖面图. (a~c) 空白NCM811-LGPS; (d~f) LNO包覆NCM811-LGPS[106]

Figure 10. The Operando XANES studies of SSLBs with bare and LNO-coated NCM811 cathodes during cycling: S K-edge spectra, Ni K-edge spectra, and charge/discharge profiles of (a-c) bare-NCM811- LGPS, (d-f) LNO coated NCM811-LGPS. Reproduced with permi- ssion[106]. Copyright 2020, American Chemical Society

图11. 原位XRD测量[108]. (a) 原位XRD装置示意图. (b) 初始Li/S和TG-Li/S电池中Li2S的相演化, 表明Li2S不能在TG-Li的金属锂表面沉积

Figure 11. (a) Schematic of in situ XRD investigation. (b) Li2S phase evolution in the bare Li/S and the TG-Li/S battery, demonstrating that Li2S cannot deposit on the metallic Li surface of TG-Li. Reproduced with permission[108]. Copyright 2018, American Chemical Society

图12. 原位NDP测量[112]. (a) Li/石榴石/碳纳米管不对称电池. (b) Li/石榴石/Li对称电池. 在不同时间背景校正后(1, 4)、在一个电镀溶解周期内(2, 5)的典型NDP谱和循环过程中每5 min采集一次NDP光谱的二维投影(3, 6)

Figure 12. In situ NDP measurement. (a) The Li/garnet/CNT asymmet- ric cell and (b) the Li/garnet/Li symmetric cell while cycling. Typical NDP spectra after background calibration at different times (1, 4) and during one plating-stripping cycle (2, 5). (3, 6) 2D projection of NDP spectra collected every 5 min during cycling. Reproduced with permiss- ion[112]. Copyright 2017, American Chemical Society

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固态锂电池电极过程的原位研究进展

In Situ/Operando Advances of Electrode Processes in Solid-state Lithium Batteries

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