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Condens. Matter 2020, 5, 75 5 of 28 contact and ensured a hermetic seal [45]. The very first cell used for transmission studies was developed by Gustafsson et al. in 1992 using a “coffee bag” type cell to study a Li|polymer-salt electrolyte|V6O13 battery. The in-situ cell is shown in Figure 1c and was composed of a thin layer of metallic lithium and a V6O13 electrode coated on a nickel foil in a polymer-coated aluminum-foil bag [26]. The in-situ cell allowed the authors to monitor the structural changes associated with solid-state reactions under realistic electrochemical conditions. Amatucci and co-workers characterized the structure of a LixCoO2 electrode at voltages greater than 5 V without any beryllium corrosion, with the use of an in-situ cell with an air gap between the Be window and the electrochemically active part of the cell [27]. The schematic of the cell is shown in Figure 1d. A complete historical overview of the developments of designs and technical details of electrochemical cells used for in situ X-ray studies is out of the scope of this review, but has been largely summarized by Morcrette et al. [11]. Condens. Matter 2020, 5, x 5 of 30 Figure 2. Experimental set up of the experiment, ED-XRD data obtained from 3 different coin cells Figure 2. Experimental set up of the experiment, ED-XRD data obtained from 3 different coin cells (A) not discharged and (B,C) discharged to 0.5 electron equivalents at C/1440 at two different (A) not discharged and (B,C) discharged to 0.5 electron equivalents at C/1440 at two different positions positions and (D,E,F) discharged to 0.5 electron equivalents at C/168. and (D–F) discharged to 0.5 electron equivalents at C/168. NOonweaodfatyhse,ftihrsetmino-stitaudXoRpDtedceclelsllwcoansfidgeuvrealotipoends ainre1t9y7p8icbayllCyhbieasnpeollkieancodinhicsecllos-auntdhoprosufcohrctehlels, wsthuidchyaorfeamLoid/TifiiSe2dcwelilt.hTchoeaxceiallhwoalsesdceosvigenredwfoirthaXc-ornayvetnratinosnpaalrBenratgtgh–inBrfielnmtanpolydmifferracwtoimndeotewrs twoocorknifinngeinthrefelelecctitornolmytoed[e1,3c,4o6m].pFoisgeudroef3aa5,b0μshMo-wthtiwckoBexwaminpdloews,oafnmdoadTifiefeldonc/oailnumceilnlusmanbdopdoyuinch caellpsa,raelslpelecptilvateelyc.oCnofingucrealltsiocnan[2a5ls].oTbheemsocdheifimeadtiwciothfathtehicneglllaissswhoinwdnowin(1F0ig0uμrme-1tbh.icTkh),ewahuitchocrasn bme ofinxietodrweditthea pdoisloyredtherylienntehfeoTilihS2eactaetdhoadtehdiguhritnegmdpiesrcahtaurrgee,(4w53hiKch) [w47a]s, allsotewpi-ncghanmgeoirne ubantitfeorrym srteascekarpcrhesastutrheawttitmher,esipneccet,tinotphoelypmreevriofiulmswso[4r8k]s.,eSlteacntrdoadredspwoeurcehsecpelalrsawteidthaonudtamnoaldyizfiecdateiox-nsictuan before and after the electrochemical polarization [44]. However, this preliminary cell was not exempt also be used in combination with synchrotron-based high-energy X-rays in transmission geometry: from limitations; only 10% of the electrode was analyzed, due to the penetration depth of the X-rays high-energy photons are able to fully penetrate the cell, obtaining a 2D diffraction patterns under through the cell window (50 μ M-thick) and the electrode (700 μ M-thick). After this first experiment, more realistic conditions with respect to those obtained using a custom cell [49,50]. An alternative a large series of cell configurations were tested by different groups. Dahn and co-workers analyzed configuration is given by Argonne’s multipurpose in situ X-ray (AMPIX) cell, shown in Figure 3c and structural changes in LixTiS2 using an in-situ cell composed of two stainless steel cases, each one with characterized by a cup-shaped body, two X-ray transparent windows and a flat annular gasket which a Be window coated with the electrode. An electrolyte-soaked separator and a polypropylene gasket prevented electrical contact and ensured a hermetic seal [45]. The very first cell used for transmission studies was developed by Gustafsson et al. in 1992 using a “coffee bag” type cell to study a Li|polymer-salt electrolyte|V6O13 battery. The in-situ cell is shown in Figure 1c and was composed of a thin layer of metallic lithium and a V6O13 electrode coated on a nickel foil in a polymer-coated aluminum-foil bag [26]. The in-situ cell allowed the authors to monitor the structural changesPDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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