Recent advances in battery characterization using in situ XAFS, SAXS, XRD, and their combining techniques: From single scale to multiscale structure detection

Abstract

Revealing and clarifying the chemical reaction processes and mechanisms inside the batteries will bring a great help to the controllable preparation and performance modulation of batteries. Advanced characterization techniques based on synchrotron radiation (SR) have accelerated the development of various batteries over the past decade. In situ SR techniques have been widely used in the study of electrochemical reactions and mechanisms due to their excellent characteristics. Herein, the three most wide and important synchrotron radiation techniques used in battery research were systematically reviewed, namely X‐ray absorption fine structure (XAFS) spectroscopy, small‐angle X‐ray scattering (SAXS), and X‐ray diffraction (XRD). Special attention is paid to how these characterization techniques are used to understand the reaction mechanism of batteries and improve the practical characteristics of batteries. Moreover, the in situ combining techniques advance the acquisition of single scale structure information to the simultaneous characterization of multiscale structures, which will bring a new perspective to the research of batteries. Finally, the challenges and future opportunities of SR techniques for battery research are featured based on their current development.

Fine Structure and Electrochemical Performance Investigations of Spherical LiMn0.6Fe0.4PO4/C Cathode Material Synthesized via a Spray-Drying Route at Various Calcination Temperatures

“…This shift signifies a dominant role of iron in the charge compensation mechanism. Consistent with the behavior observed for manganese, iron would not oxidize to the tetravalent state which could provoke Jahn–Teller distortions. , …”

“…Consistent with the behavior observed for manganese, iron would not oxidize to the tetravalent state which could provoke Jahn−Teller distortions. 33,34 Because the d-electron orbitals of Fe were not filled, they were partially characterized using the Mossbauer spectroscopy method, and ex-Fe-MS tests were performed on ex-Fe-MS at various states of charge and discharge. Figure 10a−d shows Fe-MS measurements of the electrodes of the cell after charging it to 3.8 and 4.25 V and discharging it again to 2 V after cycling the cell for 2 revolutions, and the charging and discharging of the samples was compared to the original samples (Table 4).…”