Lab‐Scale In Situ X‐Ray Diffraction Technique for Different Battery Systems: Designs, Applications, and Perspectives

Abstract

In order to meet the growing demands of electric vehicles and portable devices, the electrochemical performance of rechargeable batteries is required to be further optimized. Above all, it is of vital importance to understand the reaction mechanism of batteries under working states, which requires a direct observation of the complicated reaction process. Thus, in situ X‐ray diffraction (XRD) techniques have been employed in the charge and discharge process to realize real‐time monitoring and provide on‐site information of structural evolutions and phase transitions within electrode materials. In this review, a detailed summary of lab‐scale in situ X‐ray diffraction techniques is given and compared with in situ synchrotron XRD at the same time. First, four typical in situ reaction mechanisms are presented and their distinctive characteristics are introduced in detail. Second, the practical applications of in situ X‐ray diffraction in different battery systems are described with examples after extensive collections. In addition, the design of in situ cells and some noteworthy experimental details in actual testing are also mentioned. Finally, the further development direction of in situ X‐ray diffraction techniques is well prospected.

A review of hard carbon anode: Rational design and advanced characterization in potassium ion batteries

“…It is well known that in situ/operando characterization techniques are ideal to monitor the dynamic phase transition, intermediate stages, solid–electrolyte interphase formation, side reactions, chemical environment changes, ion transport properties, and structural evolution of KIBs during potassiation and depotassiation 125,126 . The frequently used in situ techniques include insitu XRD, 127 Raman spectroscopy, 53 NMR spectroscopy, 94 X‐ray absorption near‐edge structure (XANES), 128 FTIR, 129 atomic force microscopy (AFM), 130 transmission X‐ray microscopy, 131 TEM, SEM, and so on 132 .…”

Confining TiO2 Nanotubes in PECVD-Enabled Graphene Capsules Toward Ultrafast K-Ion Storage: In Situ TEM/XRD Study and DFT Analysis

“…4 b. In general, the constant signals located at 44.2° and 46.0° are related to the BeO and Be window, respectively [ 44 ]. In the meantime, the dominant peak (~ 44.8°) of B-phase TiO 2 (60-1) shows almost no change in either position or intensity during the entire charge–discharge process, while the A-phase TiO 2 (004) at ~ 38.7° displays slight shifts toward the low-angle side upon discharge, indicative of the lattice expansion along the A [004] direction upon potassiation, substantiating the occurrence of a K-ion intercalation reaction [ 45 ].…”

New types of hybrid electrolytes for supercapacitors

“…In addition to the conventional techniques such as Raman spectroscopy and the simulation methods such as DFT calculation, in-situ characterization techniques are very useful to study the internal mechanisms of the hybrid electrolyte systems. Some in-situ characterization techniques such as in-situ Raman, in-situ transmission electron microscopy (TEM) and in-situ X-ray diffraction (XRD) have been developed to study lithium ion batteries, electrocatalysis and other electrochemical materials [112][113][114][115], which can also be used to systematically explore the internal reaction mechanism of the new type of hybrid electrolytes in SCs. Taking in-situ XRD for example, put the electrode material of lithium ion batteries into an in-situ XRD cell, which connects with X-ray diffractometer and battery test instrument, the phase transitions and the structural changes within electrodes can be monitored real-time [115].…”

“…Some in-situ characterization techniques such as in-situ Raman, in-situ transmission electron microscopy (TEM) and in-situ X-ray diffraction (XRD) have been developed to study lithium ion batteries, electrocatalysis and other electrochemical materials [112][113][114][115], which can also be used to systematically explore the internal reaction mechanism of the new type of hybrid electrolytes in SCs. Taking in-situ XRD for example, put the electrode material of lithium ion batteries into an in-situ XRD cell, which connects with X-ray diffractometer and battery test instrument, the phase transitions and the structural changes within electrodes can be monitored real-time [115]. Besides the work performance of SCs such as the important factor of energy density, the cost and environmental impacts are also very important concerns in evaluating the practical application of an electrolyte.…”