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Batteries 2022, 8, 6 10 of 18 2.5. Analysis of Electrode-Electrolyte Interphase To better understand the mechanisms for the apparently different behaviour between the three binders, we carried out electrochemical impedance (EIS) studies as well as SEM Batteries 2022, 8, x FOR PEER REVIEW and XPS characterization of the cycled electrodes. 10 of 19 EIS results, shown in Figure 6, show the evolution of internal resistances. EIS data of uncycled cells, cells after formation (3 full charge-discharge cycles at a slow C-rate), and after 50 cycles at 1 C (175 mA/g) are shown. Two arcs are observed for all electrodes. The after 50 cycles at 1 C (175 mA/g) are shown. Two arcs are observed for all electrodes. The first corresponds to SEI resistance while the second to charge transfer processes [52,53], first corresponds to SEI resistance while the second to charge transfer processes [52,53], although the precise interpretation of these types of EIS results is still being disputed and although the precise interpretation of these types of EIS results is still being disputed and mmigihgthbtebemmoroereamambibgiugouuouss[5[45,45,5]5.]A.AssGGabaebresrcseckeketeatla.lh.ahvaeveshsohwownn[5[45]4,]i,ninsosmomeecacsaesse,st,htehe hihgihghfrfereqquueennccyyarrccanalsoccoorrreessppoonnddtotoelelcetcrotrdoed-ecu-crurernretnctolcloecllteocrtorersrisetsainstcaenrcaethrearththearn thtahne tShEeI.SEI. 1600 1400 1200 1000 800 600 400 200 00 400 800 ZRe (W) (a) 1200 1600 6000 5000 4000 3000 2000 1000 00 1000 2000 3000 4000 5000 6000 ZRe (W) (b) 2500 2000 1500 1000 500 00 500 1000 1500 2000 2500 ZRe (W) (c) Figure 6. EIS spectra of Na0.67MnO2 electrodes prepared with (a) PVDF, (b) Na alginate and (c) TBA Figure 6. EIS spectra of Na0.67MnO2 electrodes prepared with (a) PVDF, (b) Na alginate and (c) TBA alginate binders, measured 3 h after assembly of the cell, after 3 formation cycles at a slow rate and alginate binders, measured 3 h after assembly of the cell, after 3 formation cycles at a slow rate and after 50 cycles at 1 C (175 mA/g). after 50 cycles at 1 C (175 mA/g). Looking at the EIS spectra individually (Figure 6a–c), we find that the internal re- Looking at the EIS spectra individually (Figure 6a–c), we find that the internal resis- sistances of PVDF-based electrode change relatively little, with SEI resistance increasing tances of PVDF-based electrode change relatively little, with SEI resistance increasing after after formation, and charge transfer resistance slightly reducing after 50 cycles. The sec- formation, and charge transfer resistance slightly reducing after 50 cycles. The second semi- ond semicircle of the EIS spectrum of the PVDF-based electrode flattens with cycling, circle of the EIS spectrum of the PVDF-based electrode flattens with cycling, pointing to the pointing to the arising inhomogeneities, likely on the electrode’s surface. Na alginate- arising inhomogeneities, likely on the electrode’s surface. Na alginate-based Na0.67MnO2 based Na0.67MnO2 electrode undergoes significant changes, with both resistances notably electrode undergoes significant changes, with both resistances notably shrinking during shrinking during cycling. Both charge transfer and SEI resistances of TBA alginate-based cycling. Both charge transfer and SEI resistances of TBA alginate-based electrode initially electrode initially shrink similarly to the Na alginate-based electrode. However, after 50 shrink similarly to the Na alginate-based electrode. However, after 50 cycles, an increase in cycles, an increase in the SEI resistance is observed. the SEI resistance is observed. When the EIS spectra are compared for similarly aged PVDF, Na alginate, and TBA When the EIS spectra are compared for similarly aged PVDF, Na alginate, and TBA alagligniantaetebabsaesdedNNa0a.67MMnOn2Oelecltercotdroeds,ecs,ocnosnistiesntetnwt iwthitthhtehleolwoweregrrgarvaivmimeteritcricacpaapcaictyityanadnd 0.67 2 hihgihgehrerovoevrevrovlotaltgaegevavlauleuse,sN,Naalagligniantaetehahsasthtehelalragregsetstelelcetcrtordoedererseisitsatnacnec.eH.Howoweveevre,ri,tit shsrhirniknskuspuopnoncyccylcinlign,gu,lutilmtimataetleylynenaerainrigngthtahtaotfotfhtehPeVPDVDF-Fb-absaesdedelelcetcrotrdoed.eT.BTABAalgaligniantea-te- babsaesdedelelcetcrtordoededidsipslpalyasysisginginfificacnatnltylylalragrgerererseisitsatnancec.e. SESMEMmmeaesausruermemenetnstosfocfyccylceldedelelcetcrtordoedse,ss,hsohwownnininFiFgiugruere7,7i,nidnidciactaetea acocnosnisdiedrearbalbyly chcahnagnegdedelelcetcrtordoedemmoroprhpohlolgoygyofoPf VPVDDF-Fb-absaesdedelelcetcrtordoedse,sl,ikliekleylyarairsisnigngfrformoma agrgorwowththofof a apoprooruosusSESIE.IT. hTehesusrufrafcaecsesofoNf Na alagligniantaeteanadndTBTABAalagligniantaet-eb-absaesdedelelcetcrtordoedseaslaslosodidsipslpalyay vivsisbilbelessigignnssoffSEIbuiilld--up(s(suurfrafacecererseisdiudeuaenadnsdmsomotohoetrhedrgeedsgoefsgorafignrsaciannsbceanobbserovbe-d). seCrvraecdk).sCcarnacbkessceaennbiensNeeanaligninNaatea-lbgainseadtee-bleacsterdodeelescattrosdomeseastitseosm.Hesoiwteesv.eHr,otwhiesvdero,etshnisot doseesmnotot bseeamwtiodebsepraeawdidpehsepnroemadenpohne.nAolmliennaolnl,.hAowlleinvear,llt,hheoawllevlecrt,rothdesamllaeilnetcatrinodtheesir integrity, as the shape, size, or distribution of the active particles has not undergone any maintain their integrity, as the shape, size, or distribution of the active particles has not notable changes. undergone any notable changes. Na alginate TBA alginate PVDF Uncycled After formation After 50 cycles Uncycled After formation After 50 cycles Uncycled After formation After 50 cycles -ZIm (W) -ZIm (W) -ZIm (W)PDF Image | Na-Ion Batteries Tetrabutylammonium Alginate Binder
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