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Application of in-situ characterization techniques in modern aqueous batteries

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Abstract

The development of high-performance aqueous batteries calls for an in-depth knowledge of their charge–discharge redox and failure mechanism, as well as a systematic understanding of the dynamic evolution of microstructure, phase composition, chemical composition, and local chemical environment of the materials for battery. In-situ characterization technology is expected to understand and reveal the problems faced by aqueous rechargeable batteries, such as the dissolution of electrode materials, the growth of metal negative electrode dendrites, passivation, corrosion, side reactions and a series of problems. Based on this, typical in-situ characterization techniques and their basic mechanisms are summarized, including in-situ optical visualization, in-situ microscopy techniques (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 structural X-ray absorption spectroscopy (XANES)), and in-situ spectroscopy techniques (in-situ Raman spectroscopy, in-situ Fourier transform infrared (FTIR)).Moreover, some emerging techniques concerning aqueous battery research, especially gas evolution and materials dissolution issues, such as in-situ electrochemical quartz crystal microbalance (EQCM), in-situ fiber-optic sensing, in-situ gas chromatography (GC) are introduced. At last, the applications of advanced in-situ characterizations in future research of aqueous batteries are emphasized and discussed, along with some of the remaining challenges and possible solutions.

Graphical Abstract

摘要

开发高性能水系电池需要深入了解其充放电氧化还原和失效机理，并系统了解电池材料的微观结构、相组成、化学成分和局部化学环境的动态演变。原位表征技术有望了解和揭示水系电池面临的电极材料溶解、金属负极枝晶生长、钝化、腐蚀、副反应等一系列问题。在此基础上，本文总结了典型的原位表征技术及其基本机理，包括原位光学、原位显微镜技术（原位扫描电子显微镜（SEM）、原位透射电子显微镜（TEM））、 原位 X 射线技术（原位 X 射线衍射 (XRD)、原位 X 射线光电子能谱 (XPS)、原位 X射线近边吸收 (XANES)），以及原位谱学技术（原位拉曼光谱、原位傅立叶变换红外 (FTIR)）。 此外，本文还介绍了与水系电池研究有关的一些新兴技术，特别是对于研究气体演化、材料溶解等问题，如原位电化学石英晶体微分天平（EQCM）、原位光纤传感、原位气相色谱法（GC）等。最后，本文强调并讨论了先进的原位表征技术在未来水系电池研究中的应用，以及仍然存在的一些挑战和可能的解决方案

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Fig. 1

Reproduced with permission from Ref. [46]. Copyright 2022, Wiley. In-situ investigations of Zn deposition by optical microscopy in Zn/Zn cells: images of Zn-electrolyte interface region in b 1 mol·L−1 Zn(TFSI)2 and c Zn(TFSI)2-based eutectic solvent; d images of SEI-coated Zn-electrolyte interface region using 1 mol·L−1 Zn(TFSI)2. Reproduced with permission from Ref. [47]. Copyright 2019, Springer.; e schematic illustration of a designed electrochemical cell. Reproduced with permission from Ref. [53]. Copyright 2021, Springer. f An optical reflectometry setup for in-situ optical imaging from top-view. Reproduced with permission from Ref. [54]. Copyright 2022, Wiley

Fig. 2

Reproduced with permission from Ref. [64]. Copyright 2022, Elsevier

Fig. 3

Reproduced with permission from Ref. [71]. Copyright 2019, Wiley. b Transmission mode [72]. In-situ synchrotron XRD pattern collected during electrochemical discharge/charge of layered MnO2: c electrochemical discharge/charge profile and d in-situ XRD patterns. Reproduced with permission from Ref. [80]. Copyright 2018, Elsevier

Fig. 4

Reproduced with permission from Ref. [84]. Copyright 2021, Wiley. c Operando SXRD of Zn anode during charge process. Reproduced with permission from Ref. [93]. Copyright 2020, Wiley. Structural evolution of a negative electrode (bipyridinium–diamide triad) during the first cycle (scans 1 to 33) in d 2.5 mol·L−1 NaClO4 and e 1.25 mol·L−1 Mg(ClO4)2. Reproduced with permission from Ref. [94]. Copyright 2017, Wiley

Fig. 5

Reproduced with permission from Ref. [101]. Copyright 2022, Elsevier

Fig. 6

Reproduced with permission from Ref. [103]. Copyright 2020, American Association for the Advancement of Science

Fig. 7

Reproduced with permission from Ref. [108]. Copyright 2021, Wiley

Fig. 8

Reproduced with permission from Ref. [111]. Copyright 2022, Royal Society of Chemistry. d Schematic diagram of in-situ ATR-FTIR analysis; e in-situ ATR-FTIR spectra of an organic cathode in one discharge/charge cycle. (The change of the line color from blue to red indicates the change of the organic cathode from a discharged state to a charged state). Reproduced with permission from Ref. [114]. Copyright 2018, American Association for the Advancement of Science

Fig. 9

Reproduced with permission from Ref. [118]. Copyright 2022, Elsevier. d Operando UV–Vis spectroscopy results of electrolyte during charge process of ZIABs. Reproduced with permission from Ref. [93]. Copyright 2020, Wiley

Fig. 10

Reproduced with permission from Ref. [120]. Copyright 2021, Wiley

Fig. 11

Reproduced with permission from Ref. [126]. Copyright 2022, Springer. Cathodic stability and H2 evolution behavior for b H2O electrolyte; and for c RME determined by LSV and operando gas pressure measurement. Reproduced with permission from Ref. [127]. Copyright 2023, Springer

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Acknowledgements

This work was financially supported by the National Key Research and Development Program of China (No. 2022YFB2404300) and the Key R&D Program of Hubei Province (No. 2022BAA028).

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  1. Department of Physics, State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, School of Materials Science and Engineering, Wuhan University of Technology, Wuhan, 430070, China

    Jia-Hao Wu, Hong-Wei Cai, Zhao-Hui Deng & Wen Luo

  2. Laboratoire de Chimie Et Physique: Approche Multi-Échelles, Des Milieux Complexes (LCP-A2MC), Institut Jean Barriol, Université de Lorraine, 57070, Metz, France

    Jean-Jacques Gaumet

  3. Department of Medicinal Chemistry, Hubei College of Chinese Medicine, Jingzhou, 434020, China

    Yu Bao

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Wu, JH., Cai, HW., Deng, ZH. et al. Application of in-situ characterization techniques in modern aqueous batteries. Rare Met. (2024). https://doi.org/10.1007/s12598-024-02689-7

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