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understood. It is proposed that at lower voltages the layered transition metal oxide structure of the cathode is active and at higher voltages the monoclinic Li2MnO3−structure is activated [83,84]. However, in the BCDI experiment no two-phase behaviour was observed and so it is proposed that there is anionic activity that results in the higher capacity of lithium rich layered transition metal oxide cathodes. Dislocations play a big part in providing a ‘pipeline’ for oxygen vacancy mobility. Condens. Matter 2020, 5, 75 12 of 28 With the addition of further studies, including imaging and spectroscopic techniques oxygen activity within cathode materials could be better understood [80]. Figure 7. Rendering of cathode active material from the operando measurements during charge (a) at Figure 7. Rendering of cathode active material from the operando measurements during charge (a) at 4.0 V—a dislocation free crystal, (b) at 4.3 V and the presence of two dislocations, (c) 4.3 V and a 4.0 V—a dislocation free crystal, (b) at 4.3 V and the presence of two dislocations, (c) 4.3 V and a Figure 80. Ulvestad et al. suggested that BCDI could be a useful tool for defect engineering, where formed dislocation network. The arrow labelled q indicates the direction of the X-ray scattering vector, designing the defect system could be used to generate desirable properties. Since BCDI is a technique perpendicular to the atomic layers [80]. that allows for nanoscale resolution of defects under operando conditions it is uniquely powerful for this purpose [85]. Ulvestad et al. suggested that BCDI could be a useful tool for defect engineering, where designing the defect system could be used to generate desirable properties. Since BCDI is a technique that Ulvestad et al. suggested that BCDI could be a useful tool for defect engineering, where allows for nanoscale resolution of defects under operando conditions it is uniquely powerful for this designing the defect system could be used to generate desirable properties. Since BCDI is a technique purpose [85]. that allows for nanoscale resolution of defects under operando conditions it is uniquely powerful for tOhivsepruarllp,oBsCeD[8I5]i.samethodthathasyettofullybetakenadvantageofforoperandoexperimentsof battery mOavteraiall,sB. CTDheIyisaaremdeitffihocdutlhtaetxhpaesriymetetnotsfutlolypbeerftoakrmenbaudtviatnitsageessoefnftoiarlotpoeruanddoeerxsptaenridmdenistsorder of battery materials. They are difficult experiments to perform but it is essential to understand at the nanoscale to elucidate degradation mechanisms and lead on to design improvements. BCDI is a disorder at the nanoscale to elucidate degradation mechanisms and lead on to design improvements. valuable tool for visualizing events at the nanoscale as it can directly image the interior of particles of BCDI is a valuable tool for visualizing events at the nanoscale as it can directly image the interior of this size [80]. The Kapton windowed cells used in these examples, however, may not be suitable for particles of this size [80]. The Kapton windowed cells used in these examples, however, may not be longer duration cycling (for the reasons previously outlined) and thus a more robust operando cell suitable for longer duration cycling (for the reasons previously outlined) and thus a more robust design could yield similar improvement in understanding of the evolution of structural defects with operando cell design could yield similar improvement in understanding of the evolution of structural longer cycle lives as those obtained using the long duration PXRD [65]. Developments are also being defects with longer cycle lives as those obtained using the long duration PXRD [65]. Developments made both in computational power and increasing the photon flux allowing for BCDI to become a are also being made both in computational power and increasing the photon flux allowing for BCDI crucial probe for electrochemical studies [86]. to become a crucial probe for electrochemical studies [86]. 5. XRD Coupled with Other Techniques 5. XRD Coupled with Other Techniques TheTchoemcpolmexpilteyxiotyfopfhpehneonmomeneanaoocccuurrriing in LIBsdurrininggththeelelcetrcotrcohcehmeimcalicraelacrteiaocnt,ioand, athned the heterhoegternoegietniesitieosf obfatbtaetrtyerymmataetreirailasl,s, oofftten make iitt neecceessasrayrytotousuesevavriaoruisoucsomcpolmempelenmtareyntary The combination of XRD and X-ray absorption spectroscopy (XAS) is usually used to investigate phase transitions and reaction kinetics during the ionic intercalation/deintercalation of electrode material [51,54]. Operando XAS, including X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) has extensively been used to study the oxidation state variations of specific elements and the evolution of interatomic distances in the electrode materials as a function of state of charge [87]. Sottman and co-authors presented an electrochemical cell for operando quasi-simultaneous XRD and absorption XANES and EXAFS measurements at the Swiss Norwegian Beamlines (SNBL) at the European Synchrotron (ESRF, Grenoble, France) [88]. The proposed cell, shown in Figure 8a (scheme on the right), has been characterized by metallic pistons with Kapton characterization techniques in concert. Events such as phase transformation, ion diffusion, surface characterization techniques in concert. Events such as phase transformation, ion diffusion, surface modification, and charge transfer at the electrode, can require multi-operando and multi-scale measurements, combining together scattering, imaging and spectroscopy.PDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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