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Condens. Matter 2020, 5, 75 15 of 28 co-authors to study the non-equilibrium phase transition in layer structured NMC LiNi1/3Mn1/3Co1/3O2 cathodes during cycling. The experiment was performed at the beamline X14A of the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory (BNL). A different three-phase transition behaviour was demonstrated by in-situ XRD; the 003 diffraction peak evolution of NMC electrode during the first charge is observable in Figure 10a; thanks to ex-situ scanning-TEM analysis, the authors observed the coexistence of an abnormal Li-poor region with tetrahedral Li occupation and a normal Li-rich region with octahedral Li occupation. Figure 10b shows TEM images taken along Condens. Matter 2020, 5, x 16 of 30 Figure 10. (a) 003 diffraction peak evolution of NMC cathode during the first charge; (b) TEM image Figure 10. (a) 003 diffraction peak evolution of NMC cathode during the first charge; (b) TEM image taken along the [110] zone axis of the NMC electrode after 55 s charging at the current rate of 30 C, taken along the [110] zone axis of the NMC electrode after 55 s charging at the current rate of 30 C, with zoom-in image of the areas marked with yellow and pink squares, respectively [95]. with zoom-in image of the areas marked with yellow and pink squares, respectively [95]. Transmission X-ray microscopy (TXM) conducted in advanced synchrotron facilities is also a the 110 zone axis [95]. Transmission X-ray microscopy (TXM) conducted in advanced synchrotron facilities is also a powerful tool to characterize battery materials with high spatial resolution (~30 nm using hard powerful tool to characterize battery materials with high spatial resolution (~ 30 nm using hard X- X-rays) and providing a large field of view (~tens of μm), which is ideal for tomographic imaging rays) and providing a large field of view (~ tens of μM), which is ideal for tomographic imaging in in kinetic studies [5,96]. Li2MnO3·LiMO2 electrodes were investigated with operando TXM coupled kinetic studies [5,96]. Li2MnO3·LiMO2 electrodes were investigated with operando TXM coupled with with neutron powder diffraction by Chen and co-authors. Analysing the morphological evolution of neutron powder diffraction by Chen and co-authors. Analysing the morphological evolution of particles during the first charge/discharge cycle, they observed how the morphological evolution of particles during the first charge/discharge cycle, they observed how the morphological evolution of particles is directly correlated to electrochemical function. Particle cracking was revealed to be initiated particles is directly correlated to electrochemical function. Particle cracking was revealed to be during further charge to 4.7 V vs. Li+/Li during the concurrent two-phase reaction of the LiMnO2 intensified during further charge to 4.7 V vs. Li+/Li during the concurrent two-phase reaction of the by the solid-solution reaction of the LiMnO2 phase on charge to 4.55 V vs. Li+/Li and intensified initiated by the solid-solution reaction of the LiMnO2 phase on charge to 4.55 V vs. Li+/Li and phase, involving the largest lattice change of any phase, and oxygen evolution from the Li2MnO3 phase. LiMnO2 phase, involving the largest lattice change of any phase, and oxygen evolution from the Chen and co-workers employed scanning transmission X-ray microscopy (STXM) at the beamline 5.3.2 Li2MnO3 phase. Chen and co-workers employed scanning transmission X-ray microscopy (STXM) at at Advanced Light Source (ASL) (Berkeley, USA) to image the local state-of-charge (SOC) and particle the beamline 5.3.2 at Advanced Light Source (ASL) (Berkeley, USA) to image the local state-of-charge morphology of a LixFePO4 (LFP) electrode in a coin cell during operando, revealing the particle by (SOC) and particle morphology of a LixFePO4 (LFP) electrode in a coin cell during operando, particle SOC pathway [97,98]. They observed that the active population depends strongly on the C-rate, revealing the particle by particle SOC pathway [97,98]. They observed that the active population exhibiting particle-by-particle-like behaviour at low rates and increasingly concurrent behaviour at depends strongly on the C-rate, exhibiting particle-by-particle-like behaviour at low rates and high rates [98]. increasingly concurrent behaviour at high rates [98]. TXM is extensively used in combination with XANES for their ability to achieve spatially resolved TXM is extensively used in combination with XANES for their ability to achieve spatially analysis of chemical phases and oxidation state of NMC materials, for instance [99], or in Li-S batteries resolved analysis of chemical phases and oxidation state of NMC materials, for instance [99], or in Li- studies [100]. However, the coupling of TXM and XRD—conducted concurrently during operando S batteries studies [100]. However, the coupling of TXM and XRD—conducted concurrently during conditions—represents a powerful tool for LIB analysis since it can give information about structural operando conditions—represents a powerful tool for LIB analysis since it can give information about and morphological changes in the battery during operation [101,102]. Villevieille and co-authors structural and morphological changes in the battery during operation [101,102]. Villevieille and co- analysed the lithiation dynamics in negative electrodes composed of Ti containing Sb particles [103]. authors analysed the lithiation dynamics in negative electrodes composed of Ti containing Sb corresponds to unreduced 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 The operando XRD and TXM were performed at the MS-powder (X04SA) and at the TOMCAT particles [103]. The operando XRD and TXM were performed at the MS-powder (X04SA) and at the bTeOamMlCinAesTabtetahme lSiwneissatLtihgehtSwSoiussrcLeig(ShLt S)ou(Vrcileli(gSeLnS,)S(wVitllziegrelnan, Sdw),irtezseprleacntidv)e,lrye.sTphecetiavuetlhyo.rTshoebasuetrhvoerdsa cobres-esrhveldl laitchoiareti-osnhepllrolictehsiastwiohnicphroincedsuscweshcicrhacikndgurocwesthcranckdgvraorwietshwainthd pvariteicslewsiitzhepaanrdticmleosripzheoalnodgy. Fmigourrpeh1o1loagsyh.oFwigsutrhee1o1paersahnodwosXthReDo(pueprpanerdogrXapRhD) o(ubptapienredgrfaoprh1)4osbctaaninsetdakfeonra1t4resgcaunlasrtianktenrvatls druergiunlgarthienfiterrsvtaelsecdtruorcihnegmtihceal frierdstucetlieocntr(orcehperemsiecnatledreidnutchteiomnid(rdelpe)r.eSsecnante0dcoinrrethspeomndidsdtoleu).nrSecdaunce0dPDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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