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Condens. Matter 2020, 5, 75 16 of 28 particles in the electrochemical cell prior to cycling at open circuit conditions. The bottom image represents a colour map corresponding to the X-ray linear attenuation coefficients, which is linked to mass density and elemental composition scale of the four steps during the electrochemical reduction: pristine Sb-Ti particle (step 0), SEI layer growth (step I), beginning of the Sb lithiation through a core–shell process (step II), phase transition which induces particle fracture and ejection of Ti (step III), and continues fracture and volume expansion (step IV). Figure 11b shows the X-ray tomograms of selected particles presenting experimental evidence for a core–shell phase-evolution process and for Condens. Matter 2020, 5, x 17 of 30 unequal reduction kinetics in different particles. Figure 11. (a) operando XRD (upper) obtained for 14 scans during the first electrochemical reduction Figure 11. (a) operando XRD (upper) obtained for 14 scans during the first electrochemical reduction represented in the middle; colour map of the X-ray linear attenuation coefficients (bottom): the colour represented in the middle; colour map of the X-ray linear attenuation coefficients (bottom): the colour red can be associated with the high-density phases (i.e., Sb and TiSb2 ), the yellow–green with low-density red can be associated with the high-density phases (i.e., Sb and TiSb2), the yellow–green with low- phases (i.e., Li Sb and Li Sb), and the blue regions with weakly absorbing components of the electrode 23 density phases (i.e., Li2Sb and Li3Sb), and the blue regions with weakly absorbing components of the (i.e., carbon black, polymeric binder, and electrolyte); (b) X-ray tomograms of selected particles recorded electrode (i.e., carbon black, polymeric binder, and electrolyte); (b) X-ray tomograms of selected every 24 min during lithiation. Scale bar: 20 μM. particles recorded every 24 min during lithiation. Scale bar: 20 μM. 6. XRD-CT 6. XRD-CT While synchrotron XRD has been successfully applied to study changes to battery materials’ While synchrotron XRD has been successfully applied to study changes to battery materials’ lattice parameters, phase transformation mechanisms, site occupancy or changing atomic position, lattice parameters, phase transformation mechanisms, site occupancy or changing atomic position, computed tomography (CT) has been shown to be an excellent tool to analyse volumetric changes and computed tomography (CT) has been shown to be an excellent tool to analyse volumetric changes resulting crack formation, or mechanical degradation mechanisms in electrodes upon electrochemical and resulting crack formation, or mechanical degradation mechanisms in electrodes upon cycling [104]. Thanks to the high brilliance X-rays generated by synchrotrons, X-ray scattering coupled electrochemical cycling [104]. Thanks to the high brilliance X-rays generated by synchrotrons, X-ray simultaneously with tomography analysis allows for the acquisition of spatially resolved signal from scattering coupled simultaneously with tomography analysis allows for the acquisition of spatially the interior of an object under working conditions. XRD-CT experiments are usually performed using resolved signal from the interior of an object under working conditions. XRD-CT experiments are a micro pencil beam (2–100 μm2) which maps a 2D cross section translating the sample perpendicularly usually performed using a micro pencil beam (2−100 μM2) which maps a 2D cross section translating to the beam. This process is repeated several times at angular increments until the sample has been the sample perpendicularly to the beam. This process is repeated several times at angular increments rotated by at least 180◦. The diffraction data is recorded while translating and rotating the sample, until the sample has been rotated by at least 180°. The diffraction data is recorded while translating and then radially integrated. The result is a sinogram which is back-projected via a suitable algorithm and rotating the sample, and then radially integrated. The result is a sinogram which is back- to a square pixel image where each pixel comprises a full diffraction pattern [60]. The technique has projected via a suitable algorithm to a square pixel image where each pixel comprises a full diffraction been first demonstrated on a synchrotron facility by Bleuet et al. adopting Harding’s original CT pattern [60]. The technique has been first demonstrated on a synchrotron facility by Bleuet et al. approach, but is now becoming routine [105]. adopting Harding’s original CT approach, but is now becoming routine [105]. Taking advantage of XRD-CT’s ability to spatially resolve phenomena is the work performed by Daemi et al. which analyzed the change in unit cell parameters upon cycling, allowing for heterogeneities within the cell to be studied at multiple scale lengths, from particle to electrode [106]. A multiscale approach is necessary in order to understand the phenomena at all levels and how they materialize into full-cell degradation. The pencil beam used for XRD-CT also leads to high spatial resolution in point diffractionPDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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