Three-Dimensional Reconstruction and Analysis of All-Solid Li-Ion Battery Electrode Using Synchrotron Transmission X-ray Microscopy Tomography

Li, Tianyi; Kang, Huixiao; Zhou, Xinwei; Lim, Cheolwoong; Yan, Bo; Andrade, Vincent De; Carlo, Francesco De; Zhu, Likun

doi:10.1021/acsami.7b18962

Cited by 29 publications

(29 citation statements)

References 31 publications

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“…Synchrotron‐based XRM, such as transmission X‐ray microscopy (TXM), X‐ray tomographic microscopy (XTM), and X‐ray fluorescence microscopy (XRF), provides the opportunities for directly visualizing the battery materials, and therefore offers the straightforward information of the microstructure and chemical composition. [7c,18] Depending on the setup of the imaging systems and the corresponding principles of the information extraction, there are mainly two different categories, i.e., real‐space imaging methods and reciprocal space imaging methods. The acquired data using real‐space imaging methods are straightforward to visualize, but the ultimate spatial resolution is very dependent on the quality of the X‐ray optics used in the imaging system .…”

Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

“…The 3D spatial structure of the sample can then be constructed using 2D XTM images, which makes the visualization and quantification of the 3D microstructure possible. [18b,22] For example, by tracking the 3D structural/chemical evolution of Sn electrodes during the electrochemical cycles using in situ/operando XTM, Wang et al elucidated a superior (de)sodiation equilibrium in sodium ion batteries. [18b] In contrast, XRF is a combination of spectroscopic analysis with imaging methods in either full‐field or scanning modes, which can resolve the distribution of different elements and chemical species.…”

Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

“…[18b,22] For example, by tracking the 3D structural/chemical evolution of Sn electrodes during the electrochemical cycles using in situ/operando XTM, Wang et al elucidated a superior (de)sodiation equilibrium in sodium ion batteries. [18b] In contrast, XRF is a combination of spectroscopic analysis with imaging methods in either full‐field or scanning modes, which can resolve the distribution of different elements and chemical species. It should be noted that the XRF is also compatible with the tomography technique to resolve the 3D spatial structure …”

Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

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Deciphering the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando Synchrotron‐Based Characterization Techniques

Yan

Cheng

Zhang

et al. 2019

Advanced Energy Materials

111

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have been the dominant energy storage devices for portable electronic devices and electric vehicles since 1990s. [1] However, the highest energy densities of LIBs are approaching their theoretical limits, hindering the widespread application of LIBs in a variety of emerging mobile transport applications. Therefore, advanced battery systems with high energy density and low cost that go beyond conventional LIBs are highly required. [2] Among different candidates of nextgeneration energy storage systems, lithium-sulfur (Li-S) batteries have attracted remarkable attention because of the high theoretical specific capacity of 1675 mAh g −1 and specific energy density of 2600 Wh kg −1 . [2g,3] Moreover, sulfur also has the advantages of nature abundance, nontoxicity, environmental benignity, and low cost. Therefore, Li-S batteries are considered as one of the most-promising candidates for next-generation electrochemical energy storage systems for electric vehicles and large-scale grids. [2b,c,4] For a typical Li-S battery, it is composed of lithium metal anode, organic electrolyte, and sulfur composite cathode (Figure 1a). During the discharge process, sulfur is reduced first to high-order polysulfides Li 2 S x (4 ≤ x ≤ 8) and then to low-order polysulfides Li 2 S x (1 ≤ x < 4). For Li-S batteries using ether-based organic electrolyte, there are two discharge plateaus at 2.3 and 2.1 V (Figure 1b), which correspond to the transformations of sulfur to Li 2 S 4 and Li 2 S 4 to Li 2 S, respectively. During the following charge process, Li 2 S is oxidized to elemental sulfur via the formation of intermediate lithium polysulfides.Despite the above-mentioned advantages, the practical application of Li-S batteries is still facing numerous challenges. For one thing, both sulfur and full discharge product Li 2 S are electronically and ionically insulating, resulting in low rate capability and low energy density. In addition, the formation and growth of Li 2 S on the surface of sulfur electrode during the discharge process can further impede the lithiation of sulfur. For another thing, the intermediate products, i.e., lithium polysulfides, have a high solubility in the organic electrolytes, resulting in the notorious "shuttle effect," low Coulombic efficiency, and passivation of the lithium metal electrode with insoluble Li 2 S/Li 2 S 2 . [2b,c,5] Since the concentration of dissolved Lithium-sulfur (Li-S) batteries have received extensive attention as one of the most promising next-generation energy storage systems, mainly because of their high theoretical energy density and low cost. However, the practical application of Li-S batteries has been hindered by technical obstacles arising from the polysulfide shuttle effect and poor electronic conductivity of sulfur and discharge products. Therefore, it is of profound significance for understanding the underlying reaction mechanism of Li-S batteries to circumvent these problems and improve the overall battery performance. Advanced characterization techniques, especially synchrot...

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Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

Section: Working Principles Of Advanced Synchrotron‐based Characterizmentioning

confidence: 99%

See 1 more Smart Citation

Deciphering the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando Synchrotron‐Based Characterization Techniques

Yan

Cheng

Zhang

et al. 2019

Advanced Energy Materials

111

View full text Add to dashboard Cite

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“…Toward this goal, single particle-level electrochemical methods have been applied to battery materials (Heubner et al, 2020). Single particle-level electrochemical measurements reveal underlying ion and electron transport processes that are fundamentally related to solid state chemistry and the solid/electrolyte interface (Nelson et al, 2017;Wolf et al, 2017;Li et al, 2018;Yu et al, 2018). Scanning probe electrochemical methods have been used to uncover heterogeneous electrochemical activity of LiFePO 4 and LiMn 2 O 4 battery particles (Kumatani et al, 2014;Tao et al, 2019).…”

Section: Introductionmentioning

confidence: 99%

Local Substrate Heterogeneity Influences Electrochemical Activity of TEM Grid-Supported Battery Particles

et al. 2021

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Understanding how particle size and morphology influence ion insertion dynamics is critical for a wide range of electrochemical applications including energy storage and electrochromic smart windows. One strategy to reveal such structure–property relationships is to perform ex situ transmission electron microscopy (TEM) of nanoparticles that have been cycled on TEM grid electrodes. One drawback of this approach is that images of some particles are correlated with the electrochemical response of the entire TEM grid electrode. The lack of one-to-one electrochemical-to-structural information complicates interpretation of genuine structure/property relationships. Developing high-throughput ex situ single particle-level analytical techniques that effectively link electrochemical behavior with structural properties could accelerate the discovery of critical structure-property relationships. Here, using Li-ion insertion in WO3 nanorods as a model system, we demonstrate a correlated optically-detected electrochemistry and TEM technique that measures electrochemical behavior of via many particles simultaneously without having to make electrical contacts to single particles on the TEM grid. This correlated optical-TEM approach can link particle structure with electrochemical behavior at the single particle-level. Our measurements revealed significant electrochemical activity heterogeneity among particles. Single particle activity correlated with distinct local mechanical or electrical properties of the amorphous carbon film of the TEM grid, leading to active and inactive particles. The results are significant for correlated electrochemical/TEM imaging studies that aim to reveal structure-property relationships using single particle-level imaging and ensemble-level electrochemistry.

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“…[2][3][4] In order to address this issue, it is necessary to understand the microstructure evolution and electrochemical performance of Sn electrodes during cycling. In recent years, several advanced techniques have been developed to investigate the microstructural evolution of anode materials during cycling in in situ and in operando cell setups, such as transmission X-ray microscopy (TXM) [5][6][7][8][9] and transmission electron microscopy (TEM). [10][11][12][13] By using synchrotron TXM, either 2D projection images or 3D microstructures have been obtained to reveal the microstructure change of Sn particles during cycling.…”

mentioning

confidence: 99%

In Situ Focused Ion Beam Scanning Electron Microscope Study of Microstructural Evolution of Single Tin Particle Anode for Li-Ion Batteries

Zhou

Cui

et al. 2019

ACS Appl. Mater. Interfaces

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Tin (Sn) is a potential anode material for high energy density Li-ion batteries due to its high capacity, safety, abundance and low cost. However, Sn suffers from large volume change during cycling, leading to fast degradation of the electrode. For the first time, the microstructural evolution of micrometer-sized single Sn particle was monitored by focused-ion beam (FIB) polishing and scanning electron microscopy (SEM) imaging during electrochemical cycling by in situ FIB-SEM. Our results show the formation and evolution of cracks during lithiation, evolution of porous structure during delithiation and volume expansion/contraction during cycling. The electrochemical performance and the microstructural evolution of the Sn micro-particle during cycling are directly correlated, which provides insights for understanding Sn-based electrode materials.

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Three-Dimensional Reconstruction and Analysis of All-Solid Li-Ion Battery Electrode Using Synchrotron Transmission X-ray Microscopy Tomography

Cited by 29 publications

References 31 publications

Deciphering the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando Synchrotron‐Based Characterization Techniques

Deciphering the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando Synchrotron‐Based Characterization Techniques

Local Substrate Heterogeneity Influences Electrochemical Activity of TEM Grid-Supported Battery Particles

In Situ Focused Ion Beam Scanning Electron Microscope Study of Microstructural Evolution of Single Tin Particle Anode for Li-Ion Batteries

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