Application of <i>in</i>-<i>situ</i> characterization techniques  in all-solid-state lithium batteries

Lu Jing-Yu; Ke Cheng-Zhi; Gong Zheng-Liang; Li De-Ping; Ci Li-Jie; Zhang Li; Zhang Qiao-Bao

doi:10.7498/aps.70.20210531

Abstract

In recent years, mobile consumer electronics and electric vehicles have been developing rapidly, and they have been hunting for lithium batteries with high energy density, high safety and stability, to alleviate the range anxiety and improve their stability over long term operations. These make all-solid-state lithium batteries very attractive and they have been under intense investigations. However, the development of high-performance all-solid-state lithium batteries requires an in-depth understanding of their charge and discharge mechanism, their degradation process, along with the evolution of the microstructures, phase compositions, chemical states and their distributions, etc., inside the battery and at the interface. This paper summarizes the basic principles, functions, and the representative advances in investigation of the dynamics and failure mechanism of electrode materials and interfaces in solid-state lithium batteries under working conditions, with typical in-situ characterization techniques, including in-situ microscopy (in-situ scanning electron microscopy (SEM), in-situ transmission electron microscopy (TEM)), in-situ X-ray techniques (in-situ X-ray diffraction (XRD)), in-situ X-ray photoelectron spectroscopy (XPS), in-situ near-edge structure X-ray absorption spectroscopy (XANES), in-situ X-ray tomography), in-situ neutron techniques (in-situ neutron diffraction (ND), in-situ neutron depth profiling (NDP)) and in-situ spectroscopies (in-situ Raman spectroscopy, in-situ nuclear magnetic resonance (NMR) and in-situ nuclear magnetic resonance imaging (MRI)), etc. We also discussed the application of future advanced in-situ characterization techniques in the investigation of all-solid-state lithium batteries.

Keywords:

Authors and contacts

1.
School of Science, Harbin Institute of Technology (Shenzhen), Shenzhen 518055, China
2.
College of Materials, Xiamen University, Xiamen 361005, China
3.
College of Energy, Xiamen University, Xiamen 361005, China
4.
School of Materials, Harbin Institute of Technology (Shenzhen), Shenzhen 518055, China
5.
College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China

Corresponding author: Li De-Ping, lideping@hit.edu.cn ; Ci Li-Jie, cilijie@hit.edu.cn ; Zhang Qiao-Bao, zhangqiaobao@xmu.edu.cn

Funds: Project supported by the Scientific Research Starting Foundation of Harbin Institute of Technology (Shenzhen), China (Grant Nos. DD29100027, DD45001022, University 20210028), the Shenzhen Steady Support Plan (Grant No. GXWD20201230155427003-20200824103000001), and the National Natural Science Foundation of China (Grant Nos. 52002094, 52122211, 52072323, 21935009, 21875196)

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图 1 典型表征技术的空间(x轴)与时间及能量(y轴)分辨率^[31]

Figure 1. Spatial (x-axis) and time/energy (y-axis) resolution of typical characterization techniques^[31].

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图 2 (a) 原位电化学扫描电子显微镜电池示意图^[34]; 在电流密度为50 μA·cm^–2下, 锂电池在沉积反应过程中的原位SEM图像 (b) 0 s; (c) 30 s; (d) 60 s; (e) 150 s; (f) 300 s; (g) 900 s; (h) 1800 s; (i) 3600 s^[34]

Figure 2. (a) Schematic diagram of the battery design for in situ electrochemical SEM^[34]; in situ SEM images of the Cu working electrode acquired at (b) 0, (c) 30, (d) 60, (e) 150, (f) 300, (g) 900, (h) 1800 and (i) 3600 s, during Li plating at the current density of 50 μA·cm^–2^[34].

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图 3 (a) 原位电化学扫描电子显微镜电池示意图^[35]; (b) 在锂电沉积过程中间隔5 min的连续SEM图像^[35]; (c) 在(b)虚线方格区域内锂电沉积过程中间隔200 s的连续SEM图像^[35]; (d) 锂棒冲破Cu CC膜的生长示意图^[35]; (e) 用蒸馏水除去电沉积锂后Cu CC膜的SEM图像^[35]

Figure 3. (a) Electrochemical cell design for the in situ SEM observation^[35]; sequential SEM images taken (b) every 5 min, and (c) every 200 s of the region in the dashed region in Figure (b)^[35]; (d) illustration of the breaking of the Cu CC film by the growth of a Li rod^[35]; (e) SEM image of the Cu CC film after removing the plated lithium with distilled water^[35].

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图 4 (a) 用于原位SEM观测的微型全固态Li-O₂电池示意图^[36]; 在锂氧电池的(b)放电和(c)充电过程中的原位SEM照片^[36]

Figure 4. (a) Schematic view of a microscale all solid-state Li-O₂ battery for in situ SEM observation^[36]; in situ SEM images of the cathode surface during the (b) discharge and (c) charge process^[36].

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图 5 (a) 固态电池中正极与固体电解质LASGTP界面附近的ADF-STEM图像^[38]; (b) 为(a)中正极在充放电过程中锂平均浓度的变化^[38]; (c), (d)分别在1−3点和4−6点锂浓度的变化^[38]; (e)−(j)在阶段A (3−18 nA·h)、阶段B (39−53 nA·h)和阶段C(充放电反应间30 min开路状态)锂分布的变化^[38]

Figure 5. (a) ADF-STEM image of the interfacial region between the cathode and solid electrolyte LASGTP in the solid-state battery^[38]; (b) evolution of the average Li concentration in the entire cathode film in Figure (a)^[38]; (c), (d) evolution of Li concentrations at points 1−3 and 4−6, respectively; (e)−(j) evolution of the Li maps at stages A (3−18 nA·h), B (39−53 nA·h), and C (open-circuit state for 30 min between the charge and discharge reactions), respectively^[38].

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图 6 (a)−(d) LATP与锂金属反应的原位TEM图^[39]; 与金属锂反应前(e)和后(f)LATP的SAED图^[39]; 在无人工层(g)和有保护层(h)下LATP|Li界面的化学-机械失效机制^[39]

Figure 6. (a)−(d) In situ TEM images of the reaction between a LATP wire and a Li metal^[39]; SAED pattern of LATP before (e) and after (f) reaction with the lithium metal^[39]; illustration of the chemomechanical failure mechanism at the LATP|lithium interface: (g) without an artificial layer^[39]; (h) with the protection layer^[39].

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图 7 (a) AFM–ETEM装置示意图^[41]; (b) TEM图像显示一个AFM悬臂梁接近锂金属的对电极^[41]; (c) TEM图像显示碳纳米管附着在扁平的AFM尖端上^[41]; (d), (e), (g) 锂晶须生长的延时TEM图像^[41]; (f) 不同生长方向锂晶须的最大应力σ_m与等效直径的关系图^[41]; (h) 8个锂晶须测试的临界压应力(当锂晶须停止生长时)与施加电压的关系^[41]

Figure 7. (a) Schematic diagram of the AFM–ETEM set-up^[41]; (b) TEM image showing an AFM cantilever approaching the counter electrode of Li metal^[41]; (c) TEM image showing a CNT attached to a flattened AFM tip^[41]; (d), (e), (g) time-lapse TEM images of Li whisker growth^[41]; (f) plot of the maximum stress σ_m versus equivalent diameter for Li whiskers with different growth directions^[41]; (h) critical compressive stress (when the growth of a Li whisker stops) versus applied voltage for eight Li whiskers tested^[41].

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图 8 用于进行(a)反射式^[48]与(b)透射式^[49]原位XRD测试的典型电池装置示意图; (c) 在一个充电-放电循环中, 利用同步辐射X光进行原位XRD表征所获得的NCM811正极XRD图谱^[49]; (d) 在指定数目的充放电循环中, 同步辐射原位XRD在1.3 Å^–1附近所获得的图谱^[49]; (e) 基于(d)中数据进行精修与物相分析所获得的各物相含量变化^[49]

Figure 8. Schematic diagram of typical setup for in situ XRD of batteries in (a) reflection mode^[48], and (b) transmission mode^[49]; (c) the in situ XRD pattern of a NCM811 cathode during a charge-discharge cycle, with the synchrotron X-ray, with local zoom in view at around 1.3 Å^–1 shown in Figure (d)^[49]; (e) evolution of relative concentration of different phases calculated based on data in Figure (d)^[49].

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图 9 (a) 典型用于原位XPS的固态电池^[60]及(b) 原位XPS系统^[57]示意图; 在Li₁₀GeP₂S₁₂ (LGPS)固体电解质上通过电化学沉积31 nm锂金属过程中, 原位XPS所检测的(c) S 2p谱、(d) Ge 3d谱, 以及(e) P 2p/Ge 3p谱, 及(f)各谱峰对应组分的相对摩尔含量随时间的变化, 包括Li₃P, Li₂S和Li–Ge合金等^[57]; (c)−(e) 中, 渐变色竖条代表典型组分的能谱峰区^[57]

Figure 9. (a) Typical solid-state battery for in situ XPS characterization^[60], and (b) Diagram of in situ XPS system^[57]; during the electrochemical deposition of 31 nm thick Li metal on LGPS solid electrolyte, evolution of the (c) S 2p spectra, (d) Ge 3d spectra, (e) P 2p/Ge 2p spectra, and (f) the evolution of relative molar concentration of phases, including Li₃P, Li₂S, and Li–Ge alloy, etc^[57]; the color stripes in Figure (c)−(e) indicate binding energy regions of typical compositions^[57].

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图 10 (a) 典型原位XANES系统^[52]及(b)对应电池结构设计示意图^[52]; 在(c)干燥空气和湿气混合物中, (d)干燥空气中, 及(e) 氩气和湿气混合物中, 120 min内对固体电解质Li₃InCl₆的原位XANES的Cl K-边谱图^[52]; (f) 对全固态电池NMC811-LGPS的原位工况XANES S K-边谱图及其(g)微分投影图^[66]; (h) Ni K-边谱以及(i)电池的充电/放电曲线^[66]

Figure 10. (a) Diagram of a typical in situ XANES system^[52], and (b) the corresponding battery structure design^[52]; Cl K-edge XANES spectra of the solid electrolyte Li₃InCl₆ acquired during its exposure for120 min in (c) mixture of dry air and moisture, (d) dry air, and (e) mixture of Ar and moisture^[52]; (f) operando S K-edge spectra with (g) first derivative mapping, and (h) Ni K-edge of a NCM811-LGPS solid state battery during a full cycle, with the charge/discharge profile shown in Figure (i)^[66]

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图 11 (a) XANES对Cu₆Sn₅负极的原位成像过程^[67]; 原位二维TXM-XANES对(b)全固态锂电池、及(c)传统基于液体电解质的锂离子电池对正极材料NCM622颗粒在充电过程中的实时成像及状态示意图^[68]

Figure 11. (a) Image formation process based on in situ XANES investigation of a Cu₆Sn₅ anode^[67]; in operando 2D TXM-XANES mapping of a NCM622 cathode particle during its charging process in (b) a solid-state battery, and (c) a Li-ion battery based on a conventional liquid electrolyte, with the corresponding schematic view included^[68].

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图 12 (a) X射线层析成像原理示意图^[70]. 相干X射线光源穿透位于可旋转台上的样品后被闪烁体转换为可见光, 光学放大后被CMOS相机拍摄成像, 然后样品旋转一个小角度进行成像, 最后对不同角度采集的投影照片重构为三维结构; (b) 原位X射线层析成像对Li|LGPS|Li电池在循环过程中LGPS片表面形貌实时监测所获得的三维结构^[72]; 原位X射线层析成像监测下, (c) 在1 mA·cm^–2电流下Li|LSPS界面随时间的变化, 其中蓝色区域表示锂金属, 棕红色区域代表界面, 黄色区域代表LSPS固体电解质^[74]; (d) Li|LSPS界面及两电极在此电流下的体积变化^[74]; (e) 电流中实际用于锂氧化的比率随界面层厚度的变化曲线^[74]; (f) Li|LSPS界面孔隙在脱锂过程中的演变过程^[74]

Figure 12. (a) Schematic diagram of the X-ray tomography process^[70]. Coherent X-rays are transmitted through the sample mounted on a rotating stage and then converted into visible light via a scintillator, the image is then optically magnified and recorded by a CMOS detector. The projected imaging process was continued during the gradual rotation of the sample, finally the data set is reconstructed into a 3D structure; (b) 3D morphology renderings of a LGPS pellet during the cycling of a Li|LGPS|Li battery with operando X-ray tomography^[72]; (c) operando X-ray tomography detected 3D growth of the Li|LSPS interface at 1 mA·cm^–2 current, with blue region indicates Li metal, brown for the interface, and yellow for LSPS solid electrolyte^[74]; (d) volumetric evolution of Li|LSPS interface and the Li at the two electrodes based on Figure (c)^[74]; (e) profile of the fraction of total current due to Li oxidation vs the thickness of the interface^[74]; (f) evolution of the voids at the Li|LSPS interface region during the stripping process^[74].

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图 13 (a) 原位3D CT-XANES测试示意图^[76]; (b) 对复合电极(LiCoO₂∶Li_2.2Co_0.8O₃ = 8∶2)在充放电过程中的原位3D CT-XANES扫描^[76]; LiFePO₄颗粒在充电过程中的(c)物相变化及(d)物相比率变化^[77]

Figure 13. (a) Schematic diagram of the operando CT-XANES system^[76]; (b) 3D mapping of the composite electrode (LiCoO₂∶Li_2.2Co_0.8O₃ = 8∶2) during the charge process^[76]; the evolution of (c) phases and (d) phase volume fraction in the LiFePO₄ particle during the charge process^[77].

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图 14 (a) NDP系统示意图^[83]; (b) 用于NDP检测非对称电池的结构设计; 对称电池中只需将此电池中的CNT正极更改为Li金属^[83]; (c) 典型Li|LLZO|Li对称电池的原位NDP谱图^[83]; (d) 为其中一个镀锂-脱锂循环过程中的NDP谱图^[83]; (e) 循环过程中对电池每5 min采集一次NDP谱后的二维(2D)投影图^[83]; (f) 在前期循环过程中, 及(g)在动态短路过程中, 用于诊断对称电池中锂枝晶短路的原位NDP谱图, 图中蓝色线表示电压, 绿色线是电量曲线, 红色线为NDP信号积分值; (h)为”动态短路”机理示意图^[83]

Figure 14. Schematic of the (a) NDP system, and (b) asymmetric battery design for NDP measurement; while only the CNT cathode needs to be replaced by Li metal in symmetric cells^[83]; typical in situ NDP spectra of a Li|LLZO|Li symmetric cell (c) at different times, and (d) during a plating-stripping cycle^[83]; (e) 2D projection of the NDP spectra acquired every 5 min during the cycling process of the symmetric cell^[83]; in situ NDP measurement for diagnosing short-circuit of a symmetric cell during the (f) predicted and (g) “dynamic short-circuit” stage of the cycling process, with blue for voltage, green for charge, and red for NDP counts, respectively^[83]; (h) schematic of the “dynamic short-circuit” mechanism^[83].

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图 15 用于进行原位拉曼检测LiCoO₂ 电极的(a)正面和(b)背面的电池示意图^[86]; 对Li_xCoO₂正极正面在(c)充电与(d)放电过程中进行原位拉曼检测的拉曼光谱^[86]

Figure 15. Schematic diagram of the battery design for in situ Raman measurement of the LiCoO₂ electrode at (a) the front side and (b) the backside^[86]; in situ Raman spectra acquired at front side of the Li_xCoO₂ cathode during (c) charging and (d) discharging process^[86].

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图 16 (a) 典型原位固态NMR电池的组成, 包括集流体、电极、隔膜以及三个由聚醚醚酮PEEK制成的电池支撑结构^[92]; (b) 组装后的原位固态NMR电池及(c)在NMR探头里的照片^[92]; 用于进行原位固态MRI而采用(d)平行线形与(e)圆盘电极的电池示意图^[92].; 对基于(f)纯硅与(g)无定形SiO (a-SiO)电极的半电池进行的 ⁷Li原位NMR波普及电压随时间的变化曲线^[92]. 对由含有锂涂层的铜圆盘电极片组成的对称电池进行的原位¹H SPRITE (T1加权单点攀升成像, 即single point ramped imaging with T1 enhancement) MRI成像图片: (h) 初始状态^[29]; 在10 μA电流下运行(i) 17, (j) 34, (k) 51 h后^[29]; 该电池在反向电流下运行 (l) 6, (m) 40, (n) 57, 及 (o) 77 h后^[29]

Figure 16. (a) Components of a typical battery for solid state NMR measurement, including current collector, electrodes, separator, and the plastic cell capsule consisting of 3 PEEK structures^[92]; (b) a NMR battery after assembly^[92]; (c) a photo of the battery in the NMR probe^[92]; schematic of symmetric cells with (d) parallel wire, and (e) disk electrodes^[92]; ⁷Li in situ NMR spectra and cell voltage during the cycling of the half-cell based on (f) pure Si, and (g) a-SiO electrode^[92]; in situ ¹H SPRITE MRI images of the lithium coated copper disk electrodes in a symmetric cell: (h) At initial state, after operation at +10 μA for (i) 17, (j) 34 and (k) 51 h; and after operation at –10 μA current for (l) 6, (m) 40 and (o) 77 h^[29].

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Application of in-situ characterization techniques in all-solid-state lithium batteries

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Corresponding author: Li De-Ping, lideping@hit.edu.cn ; Ci Li-Jie, cilijie@hit.edu.cn ; Zhang Qiao-Bao, zhangqiaobao@xmu.edu.cn

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Application of in-situ characterization techniques in all-solid-state lithium batteries

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Corresponding author: Li De-Ping, lideping@hit.edu.cn ; Ci Li-Jie, cilijie@hit.edu.cn ; Zhang Qiao-Bao, zhangqiaobao@xmu.edu.cn

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