Review on applications of synchrotron‐based X‐ray techniques in materials characterization

Understanding the complicated interplay of the continuously evolving electrode materials in their inherent 3D states during the battery operating condition is of great importance for advancing rechargeable battery research. In this regard, the synchrotron X‐ray tomography technique, which enables non‐destructive, multi‐scale, and 3D imaging of a variety of electrode components before/during/after battery operation, becomes an essential tool to deepen this understanding. The past few years have witnessed an increasingly growing interest in applying this technique in battery research. Hence, it is time to not only summarize the already obtained battery‐related knowledge by using this technique, but also to present a fundamental elucidation of this technique to boost future studies in battery research. To this end, this review firstly introduces the fundamental principles and experimental setups of the synchrotron X‐ray tomography technique. After that, a user guide to its application in battery research and examples of its applications in research of various types of batteries are presented. The current review ends with a discussion of the future opportunities of this technique for next‐generation rechargeable batteries research. It is expected that this review can enhance the reader's understanding of the synchrotron X‐ray tomography technique and stimulate new ideas and opportunities in battery research.

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Section: Fundamentals Of Synchrotron X‐ray Tomographymentioning

confidence: 99%

Synchrotron X‐Ray Tomography for Rechargeable Battery Research: Fundamentals, Setups and Applications

Tang

Yang

et al. 2021

Small Methods

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“…Synchrotron radiation sources can produce highly collimated monochromatic X-rays with high flux. Owing to these beam characteristics, structural, chemical, and physical properties can be investigated across multiple length scales 12 . In many instances, there have been applications of synchrotron radiation-based characterization, which has provided decisive answers to the physico-chemical mechanisms in MHPs that cannot be revealed by laboratory-based characterization.…”

Section: Introductionmentioning

confidence: 99%

Soft X-ray characterization of halide perovskite film by scanning transmission X-ray microscopy

Jun

Lee

Tondelier

et al. 2022

Sci Rep

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Organic–inorganic metal halide perovskites (MHPs) have recently been receiving a lot of attention due to their newfound application in optoelectronic devices, including perovskite solar cells (PSCs) which have reached power conversion efficiencies as high as 25.5%. However, the fundamental mechanisms in PSCs, including the correlation of degradation with the excellent optoelectrical properties of the perovskite absorbers, are poorly understood. In this paper, we have explored synchrotron-based soft X-ray characterization as an effective technique for the compositional analysis of MHP thin films. Most synchrotron-based studies used for investigating MHPs so far are based on hard X-rays (5–10 keV) which include various absorption edges (Pb L-edge, I L-edge, Br K-edge, etc.) but are not suited for the analysis of the organic component in these materials. In order to be sensitive to a maximum number of elements, we have employed soft X-ray-based scanning transmission X-ray microscopy (STXM) as a spectro-microscopy technique for the characterization of MHPs. We examined its sensitivity to iodine and organic components, aging, or oxidation by-products in MHPs to make sure that our suggested method is suitable for studying MHPs. Furthermore, methylammonium triiodide with different deposition ratios of PbI2 and CH3NH3I (MAI), and different thicknesses, were characterized for chemical inhomogeneity at the nanoscale by STXM. Through these measurements, we demonstrate that STXM is very sensitive to chemical composition and homogeneity in MHPs. Thus, we highlight the utility of STXM for an in-depth analysis of physical and chemical phenomena in PSCs.

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“…Owing to these beam characteristics, structural, chemical, and physical properties can be investigated across multiple length scales. [12] In many instances, there have been applications of synchrotron radiation-based characterization, which has provided decisive answers to the physico-chemical mechanisms in MHPs that cannot be revealed by laboratory-based characterization. Adhyaksa et al employed synchrotron-based nanoprobe X-ray diffraction (nano-XRD) to examine the effect of grainboundaries in MHP and veri ed that the disordered region at grain boundaries is amorphous giving rise to locally bright photoluminescence intensity, which is a quite anomalous grain boundary behavior.…”

Section: Introductionmentioning

confidence: 99%

Soft X-ray Characterization of Halide Perovskite Film by Scanning Transmission X-ray Microscopy

Jun

Lee

Tondelier

et al. 2022

Preprint

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Organic-inorganic metal halide perovskites (MHPs) have recently been receiving a lot of attention due to their newfound application in optoelectronic devices, including perovskite solar cells (PSCs) which has reached power conversion efficiencies as high as 25.5%. However, the fundamental mechanisms in PSCs, including the correlation of degradation with the excellent optoelectrical properties of the perovskite absorbers, are poorly understood. In this paper, we have explored synchrotron-based soft X-ray characterization as an effective technique for the compositional analysis of MHP thin films. Most synchrotron-based studies used for investigating MHP so far are based on hard X-rays (5–10 keV) which includes various absorption edges (Pb L-edge, I L-edge, Br K-edge, etc.) but are not suited for the analysis of the organic component in MHPs. In order to be sensitive to a maximum number of elements, we have employed soft X-ray-based scanning transmission X-ray microscopy (STXM) as a spectro-microscopy technique for the characterization of MHPs. We examined its sensitivity to iodine and organic components, aging, or oxidation by-products in MHPs to make sure that our suggested method is suitable for studying MHPs. Furthermore, methylammonium triiodide with different deposition ratios of PbI2 and CH3NH3I (MAI), and different thicknesses, were characterized for chemical inhomogeneity at the nanoscale by STXM. Through these measurements, we demonstrate that STXM is very sensitive to MHP chemical composition and homogeneity. Thus, we highlight the utility of STXM for an in-depth analysis of physical and chemical phenomena in PSCs.

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Review on applications of synchrotron‐based X‐ray techniques in materials characterization

Cited by 50 publications

References 130 publications

Synchrotron X‐Ray Tomography for Rechargeable Battery Research: Fundamentals, Setups and Applications

Synchrotron X‐Ray Tomography for Rechargeable Battery Research: Fundamentals, Setups and Applications

Soft X-ray characterization of halide perovskite film by scanning transmission X-ray microscopy

Soft X-ray Characterization of Halide Perovskite Film by Scanning Transmission X-ray Microscopy

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