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Condens. Matter 2018, 3, 36 Condens. Matter 2018, 3, x FOR PEER REVIEW 3 of 13 Condens. Matter 2018, 3, x FOR PEER REVIEW 3 of 13 MillerpFilgaunres1a.rOeninthdexlefdt sindeb,rtahcekReitest.veOldnrtehfienermigehnttsoidneF,etChoepoopwedraenrdisopXreRseDntelde.cTtrhoecmheomstircealelvparnotfile Miller planes are indexed in brackets. On the right side, the operando XRD electrochemical profile (blueliMnei)llaerndplacnoenscoarmeitnadnetxleadttincebpracrkaemtse.tOenrethveolruigthiotnsi(dre,dthsecaotpter)anadreosXhRoDwenl.ectrochemicalprofile (blue line) and concomitant lattice parameter evolution (red scatter) are shown. (blue line) and concomitant lattice parameter evolution (red scatter) are shown. 2.2. XANES Data Analysis 2.2. XANES Data Analysis 2.2. XANES Data Analysis 3 of 13 Figure 1. On the left side, the Rietveld refinement on FeCo powder is presented. The most relevant Figure 1. On the left side, the Rietveld refinement on FeCo powder is presented. The most relevant As previously reported [35,36] and indicated in Figure 2, release/insertion reaction induced a As previously reported [35,36] and indicated in Figure 2, release/insertion reaction induced a As previously reported [35,36] and indicated in Figure 2, release/insertion reaction induced a deep modification at the Fe K-edge, while the Co K-edge remained mostly unchanged. This highlights deep modification at the Fe K-edge, while the Co K-edge remained mostly unchanged. deep modification at the Fe K-edge, while the Co K-edge remained mostly unchanged. the electroactivity of the iron site with consequent electronic and structural adjustments. For instance, This highlights the electroactivity of the iron site with consequent electronic and structural This highlights the electroactivity of the iron site with consequent electronic and structural the Fe main edge shifted towards higher energies while charging, evidencing an oxidation of the metal, adjustments. For instance, the Fe main edge shifted towards higher energies while charging, adjustments. For instance, the Fe main edge shifted towards higher energies while charging, while the opposite trend was observed in the insertion process. evidencing an oxidation of the metal, while the opposite trend was observed in the insertion process. evidencing an oxidation of the metal, while the opposite trend was observed in the insertion process. FiFgiugruere2.2.XXAFS K-edgeeeevvoolulutiotinonfofrobrobthoitrhoniro(lnef(t)leafntd) acnobdaclto(briaglht t()r.iIgnhtth)e. Ibnotthoembloaytteorm, prliasytienre,, pristine, Figure 2. XAFS K-edge evolution for both iron (left) and cobalt (right). In the bottom layer, pristine, chcahragregded, ,ananddddisisccharged states speccttrraaaarereccoommpapraerdedanadndprpesrensetendtefdorfoearcehamchetmalestiatle.siTthee. Tfihgeurfiegure has charged, and discharged states spectra are compared and presented for each metal site. The figure has been adapted from reference [35]. been adapted from reference [35]. has been adapted from reference [35]. XANES analysis was performed by using a chemometric approach. MCR-ALS provides an XANES analysis was performed by using a chemometric approach. MCR-ALS provides an XANES analysis was performed by using a chemometric approach. MCR-ALS provides an additive bilinear model of pure contributions without any preexisting model or a priori information additivaedbditlivneabrilimneoadremlodfepluorfepcuorenctroinbturitbiountiosnwsiwthitohuotuatnanyypprreeexistingmoddeelloorraaprpioriroirinifionrfmoramtioantion on the system, decomposing the operando data matrix XS,W in a product of two matrices to which ontheosnystthemsy,sdtemco,mdepcosminpgostihngeothpeeorpanerdaondoadtatma matartirxixXXS,W in aproduuccttoofftwtwoommatraitcreiscetostwohwichich S,W chemical meaning can be attributed [32,37], as it follows Equation (1): chemical meaning can be attributed [32,37], as it follows Equation (1): chemical meaning can be attributed [32,37], as it follows Equation (1): XS,W = CS,F∙AW,F, (1) (1) XS,W = CS,F·AW,F, where CS,F contains the pure concentration profiles and AW,F the pure spectral components. XS,W = CS,F∙AW,F, (1) where CS,F contains the pure concentration profiles and AW,F the pure spectral components. where CS,F contains the pure concentration profiles and AW,F the pure spectral components. In this case, the MCR-ALS algorithm was applied to the whole series of operando Fe K-edge XANES spectra because of the higher variability along the W columns of the experimental XS,W matrix.PDF Image | XAFS and XRD Study of a Prussian Blue Analogue Cathode Iron Hexacyanocobaltate
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