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Batteries 2022, 8, x FOR PEER REVIEW Batteries 2022, 8, 6 C 1s Fresh Aged 294 291 288 285 282 690 688 686 684 682 660 655 650 645 640 1077 1074 1071 1068 540 535 530 Aged Binding Energy (eV) Aged Binding Energy (eV) Fresh Aged Binding Energy (eV) Aged Binding Energy (eV) Binding Energy (eV) Fresh Fresh Fresh Fresh Fresh 00 30 60 90 120 Etch time (s) Etch time (s) Etch time (s) Etch time (s) PVDF fresh Na alginate fresh PVDF cycled Na alginate cycled Etch time (s) TBA alginate fresh TBA alginate cycled 30 15 30 Fresh F 1s Mn 2p Fresh Na 1s Fresh O 1s Fresh 40 20 10 5 10 10 20 10 20 Fresh Aged 294 291 288 285 282 690 688 686 684 682 660 655 650 645 640 1077 1074 1071 1068 540 535 530 Aged Binding Energy (eV) Aged Binding Energy (eV) Fresh Aged Binding Energy (eV) Aged Binding Energy (eV) Binding Energy (eV) Fresh Fresh Aged 294 291 288 285 282 690 688 686 684 682 660 655 650 645 640 1077 1074 1071 1068 540 535 530 Binding Energy (eV) Binding Energy (eV) Binding Energy (eV) Binding Energy (eV) 25 40 50 40 60 203040 Aged Binding Energy (eV) Aged Aged Aged 20 00 30 60 90 120 00 30 60 90 120 00 30 60 90 120 00 30 60 90 120 Figure 8. XPS results of Na0.67MnO2 electrodes for fresh and aged (cycled) electrodes that have un- Figure 8. XPS results of Na0.67MnO2 electrodes for fresh and aged (cycled) electrodes that have dergone 500 charge-discharge cycles at 1 C (175 mA/g) rate—individual spectra and compositional undergone 500 charge-discharge cycles at 1 C (175 mA/g) rate—individual spectra and composi- analysis. tional analysis. NaF is a prominent part of the SEI. The XPS peak corresponding to Na-F bonding at The signal of Na changes significantly when comparing fresh and cycled TBA alginate 684.3 eV is observed for all the cycled electrodes. This is the result of the desirable decom- and PVDF alginate-based electrodes, again pointing towards a notable SEI growth, while position of FEC electrolyte additive. The peak for C-F bonding (CF2 in PVDF binder) at the Na 1s spectrum of Na alginate-based electrode stays relatively similar for fresh and 12 of 19 12 of 18 Depth profiles TBA alginate Na alginate Intensity (a. u.) PVDF Concentration (At. %) Intensity (a. u.) Intensity (a. u.) Concentration (At. %) Intensity (a. u.) Intensity (a. u.) Intensity (a. u.) Concentration (At. %) Intensity (a. u.) Intensity (a. u.) Intensity (a. u.) Concentration (At. %) Intensity (a. u.) Intensity (a. u.) Intensity (a. u.) Concentration (At. %) Intensity (a. u.) Intensity (a. u.) Intensity (a. u.) 688.2 eV is observed in fresh PVDF-based electrodes. Depth profiles of F indicate a con- aged electrodes. Peaks of ROCO2Na (1070.3 eV), Na2CO3 (1071.5 eV), and NaF (1072.8 eV) siderable amount of F trapped in the SEI. The disappearance of C-F peak at 688.2 eV in are observed for Na. After the cycling, the peaks of Na shift to the right for PVDF and the aged PVDF-based electrode again confirms the considerable thickness of the SEI, while TBA alginate-based electrodes, pointing to an increasing intensity of ROCO2Na functional the depth distribution of fluorine indicates a relatively higher fluorine content in TBA al- groups (1070.3 eV), although an appearance of NaF (1072.8 eV) is also observed. For ginate and PVDF-based electrodes compared to Na alginate-based electrodes. Na alginate-based electrode, the shift is in the other direction, signifying a considerable C1s peak can be deconvoluted into several peaks. Located at 284.8 eV is the peak prevalence of Na2CO3 (also evident from the C 1s spectrum). The Na concentration has associated with the C–C bonds of adventitious carbon and acetylene black. The peak at increased considerably after cycling for PVDF and TBA alginate-based electrodes due to approximately 285.8 eV corresponds to hydrocarbon bonding (C-H), while peaks at 287.2, the SEI growth, while it remains similar for Na alginate-based electrode due to the binder 289.2 and 290.7 eV are associated with C–O/C=O, Na2CO3 and R–CO3/CFx (x ≥ 2), respec- containing significant amount of Na. tively [49,56]. The shape and intensity of PVDF electrode changes significantly upon cy- Oxygen signal contains several bands peaking at around 530 eV and 536 eV. The latter cling, signalling a significant SEI growth, while that of Na alginate-based electrode re- is the KLL line of Na. Oxygen spectra consist of peaks at 530.1, 531.8 eV, and 532.6 eV, mains virtually unchanged. The intensity of the TBA alginate electrode’s peaks is lower corresponding to Na-O-Mn, Na2CO3, and RCH2ONa respectively. While for the PVDF and for the aged electrode, but the shape remains unchanged and signals presence of mostly Na alginate-based electrodes a large proportion comes from Na0.67MnO2 and Na2CO3, XPS C–C and C–O/C=O bonds. data from TBA alginate-based electrode contain a considerably larger number of signals Mn signal measured for most electrodes is weaker in aged electrodes. This points to coming from RCH2ONa. the formation of a SEI where Mn is not present. An exception to this is the PVDF-based To sum up, the results of the XPS point to the formation of a SEI that is Na- and Fe-lreicthroadneds,cwonhteariensthsevMenrasliogrngaalniniccyocmlepdoeulencdtsrondoet isnetensinifitehse. Tfrheeshdieslseoclturotidoens.oAf Mlthnowugash TBA alginate does not contain fluorine, judging from the XPS results, it forms Na- and F-containing compounds on its surface that are similar to those observed on PVDF-basedPDF Image | Na-Ion Batteries Tetrabutylammonium Alginate Binder
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