多空间尺度下的金属锂负极表征技术

doi:10.3866/PKU.WHXB202008091

物理化学学报 >> 2021, Vol. 37 >> Issue (1): 2008091.doi: 10.3866/PKU.WHXB202008091

所属专题：金属锂负极

多空间尺度下的金属锂负极表征技术

潘弘毅¹^,², 李泉¹, 禹习谦¹^,²^,*(), 李泓¹^,²

¹ 中国科学院物理研究所，北京 100190
² 中国科学院大学物理科学学院，北京 100049

收稿日期:2020-08-31 录用日期:2020-09-25 发布日期:2020-10-16
通讯作者: 禹习谦 E-mail:xyu@iphy.ac.cn
作者简介:禹习谦，中国科学院物理研究所研究员。2010年中国科学院物理研究所博士毕业，2010–2016年在Brookhaven国家实验室从事研究，2016年回物理研究所E01组工作。主要从事高能量密度锂离子电池与固态锂电池材料设计、二次电池材料与器件先进表征和锂电池失效分析等工作
基金资助:
国家重点研发计划(2016YFB0100100);北京市科技计划(Z191100004719001)

Characterization Techniques for Lithium Metal Anodes at Multiple Spatial Scales

Hongyi Pan¹^,², Quan Li¹, Xiqian Yu¹^,²^,*(), Hong Li¹^,²

¹ Institute of Physics, Chinese Academy of Sciences, Beijing 100190, China
² School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2020-08-31 Accepted:2020-09-25 Published:2020-10-16
Contact: Xiqian Yu E-mail:xyu@iphy.ac.cn
About author:Xi qian Yu. E-mail:xyu@iphy.ac.cn. Tel.: +86-10-82649413
Supported by:
the National Key R & D Program of China(2016YFB0100100);the Science and Technology Planning Project of Beijing, China(Z191100004719001)

摘要/Abstract

摘要：

金属锂因为其优秀的特性被认为是未来锂电池负极的最终之选。然而目前金属锂负极在旧有液态体系中的研究陷入瓶颈，在新兴固态体系中的挑战层出不穷。想要实现金属锂负极的实用化，必须加深对金属锂负极基础科学问题的认识。本文系统论述了多空间尺度下金属锂的电极行为与对应的表征技术。首先综述了多空间尺度下金属锂负极的基础科学和应用技术问题，结合近年来的工作，对全空间尺度下的先进表征手段做了梳理，分析了从原子级到宏观尺度各种表征手段的技术特点，并重点讨论了各类表征技术在研究固态体系中金属锂负极时的特点与可能的发展方向。

关键词: 锂电池, 金属锂负极, 电沉积, 表征技术, 空间尺度

Abstract:

Conventional lithium-ion batteries with graphite anode have gradually ceased satisfying demand for the rapid development of modern electric commodities, such as portable electronic devices and electric vehicles. Therefore, metallic lithium is considered the ultimate alternative anode material for future high-energy-density lithium batteries because of its excellent properties, including the highest theoretical capacity and lowest potential of available materials as well as its low density. However, research on lithium metal anodes in traditional liquid batteries has encountered impediments. Numerous studies have shown that lithium dendrites, dead lithium, solid electrolyte interphase problems, and the correlating safety hazards are the main hindrances to the practical application of liquid-based lithium metal batteries. For solid-state batteries, the challenges of lithium metal anodes continue to grow. Studies on the mechanical, thermal, chemical, and electrochemical stability of solid-state electrolyte and lithium metal anode indicate that, unlike early recognition, solid-state lithium metal batteries remain far from commercialization. Unexpected issues like lithium growth along crystal boundaries, mixed-conductivity interphase generation, and interfacial contact losses have emerged that complicate the solid-state lithium metal battery. To achieve practically applicable lithium metal anodes, it is necessary to deepen our understanding of the basic scientific issues. This review systematically discusses the electrode behaviors of lithium metal and the corresponding electrode characterization techniques at multiple spatial scales. First, the basic science and technology issues of lithium metal anodes at different scales are reviewed. Lithium electrodeposition behaviors from the atomic to the macroscale are divided into ion transportation, deposition, nucleation, crystallization, expansion and growth. Various issues are also categorized among different characteristic scales. Second, advanced characterization techniques for all spatial scales are reviewed in light of recent works. Finally, the technical characteristics of various characterization techniques from the atomic to macroscale are analyzed. Features and possible directions of improvement of various characterization techniques used to examine lithium metal anodes in solid-state batteries are highlighted. In situ observation has become a common requirement for battery characterization as it can connect macroscale phenomena to microscale mechanisms. Meanwhile, non-damaging detection techniques have faced growing demand because of the urgent need to understand the complete actual reactions at the bulk and interfaces of solid-state electrolytes and lithium anodes. The combination of techniques for different scales should provide comprehensive information to characterize lithium metal anodes and identify reasonable mechanisms for their behaviors.

Key words: Lithium battery, Lithium metal anode, Electrodeposition, Characterization technique, Spatial scale

潘弘毅, 李泉, 禹习谦, 李泓. 多空间尺度下的金属锂负极表征技术[J]. 物理化学学报, 2021, 37(1), 2008091. doi: 10.3866/PKU.WHXB202008091

Hongyi Pan, Quan Li, Xiqian Yu, Hong Li. Characterization Techniques for Lithium Metal Anodes at Multiple Spatial Scales[J]. Acta Phys. -Chim. Sin. 2021, 37(1), 2008091. doi: 10.3866/PKU.WHXB202008091

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB202008091

https://www.whxb.pku.edu.cn/CN/Y2021/V37/I1/2008091

图/表 13

图1

表1

金属锂负极相关先进表征技术基本信息表"

Characterization techniques	Minimum resolution	Field of view	Sample limits	Damage	In situ	Information	Advantages; disadvantages	References
Cryo-electronic microscopy	10^-10	10^-10–10^-5	Cryo-environment, thickness	Y	N	Near surface and cross-section morphology	Atomic resolution, air-sensitive protection; cannot do in situ observation	11, 38-42
Atomic force microscopy	10^-10	10^-9–10^-5	Surface roughness	N	Y	Surface morphology, mechanical and electronical property	Atomic resolution, abundant information; strict to surface roughness	43-47
(Scan) Transmission electronic microscopy	10^-10	10^-10–10^-5	Thickness	Y/N	Y	Near surface morphology	In situ observation; strict to thickness, damage to lithium	48-53
Electron energy loss spectroscopy	10^-9	10^-9–10^-5	Thickness	Y/N	Y	Element valence	Precise element distribution detection	41
Selected area electron diffraction	10^-8	10^-8–10^-5	Thickness	Y/N	Y	Phase	Diffraction pattern in selected area; damage to lithium	11, 38-40
Nano-X-ray computed tomography	10^-8	10^-8–10^-4	Size, X-ray attenuation coefficient	Y	Y	Surface and bulk morphology	~10 nm resolution；small field of view, not sensitive to Li, strict to sample size	54
Focused ion beam-scanning electronic microscopy	10^-7	10^-7–10^-4	Electronic conductivity	N	N	Surface and cross- section morphology	Large field of view range; surface electronic conductivity	10, 11, 26, 30, 32, 41, 55, 56
Electrochemical-scanning electronic microscopy	10^-7	10^-7–10^-4	Electronic conductivity	Y	Y	Surface morphology	In situ combination of morphology and electrochemical behavior	57, 58
Optic microscopy	10^-7	10^-7–10^-3	None	Y	Y	Near surface and side-view morphology	Direct, commonly used, high time resolution; lack of small-scale detail	9, 26, 59-64
Neutron depth profile	10^-7	10^-7–10^-3	Neutron scattering cross section	Y	Y	Element distribution in depth	Transmissive z-axis element distribution; low sensitivity in xy plane, high cost	55, 65, 66
Raman spectroscopy	10^-7	10^-7–10^-4	None	Y	Y	Component distribution	In situ surface component distribution detection; limit z-axis resolution	67
Stimulated Raman Spectroscopy	10^-6	10^-6–10^-3	None	Y	Y	Element distribution	Fast mapping speed; slightly lower spatial resolution	68
Micron-X-ray computed tomography	10^-6	10^-6–10^-2	Size, X-ray attenuation coefficient	Y	Y	Surface and bulk morphology	No limit of sample size; low Li sensitivity	69-75
X-ray photoelectronic spectroscopy	10^-6	10^-6–10^-5	Size	Y/N	Y	Element valence	Sensitive to trace element; low resolution along z-axis	76
Time of flight-secondary ion mass spectroscopy	10^-6	10^-6–10^-4	Size	Y	N	Component distribution	Element and component distribution in xy plane and z-axis; damage to sample, low spatial sensitivity	77-78
Nuclear magnetic resonance	10^-5	10^-5–10^-2	Size, skin depth	Y	Y	Element distribution	Powerful element sensitivity, non-damage bulk detection; limited by skin depth of materials	79-81
Ultrasonic transmission spectroscopy	10^-4	10^-4–10^-2	None	Y	Y	Liquid distribution	Able to detect liquid distribution, no limit of sample size; lack of exploration in solid-state battery	74
Neutron computed tomography	10^-4	10^-4–10^-2	Size, neutron scattering cross section	Y	Y	Surface and bulk morphology, element distribution	Sensitive to ⁶Li: low spatial and time resolution, high cost	82, 83

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多空间尺度下的金属锂负极表征技术

Characterization Techniques for Lithium Metal Anodes at Multiple Spatial Scales

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