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Batteries 2022, 8, 183 the fourth one, while C-FFP2 (Figure 5b) showed an initial 37% reversibility, increasing to 86% at cycle 4. As previously mentioned, the low initial reversibility was imputable to the SEI formation, while in the following cycles, the SEI reached stabilization and acted as a protective layer. In the following cycles, the broad peak in the 0.05–1 V range was associated with the reversible redox process of Na intercalation/absorption in the biochar composite (a) 30 -30 -60 -90 -30 (a) 400 300 200 100 0 The electrochemical impedance spectroscopy (EIS) was measured at open circuit 500 (b) 500 voltage (OCV) after 3 h of rest at OCV and after the cyclic voltammetric test (the electrode. 8 of 13 (b) 30 00 0.0 0.5 1.0 1.5 2.0 2.5 3.0 E vs. Na+/Na Cycle 1 Cycle 1 Cycle 2 Cycle 3 Cycle 4 0.0 0.5 1.0 1.5 2.0 2.5 3.0 E vs. Na+/Na Cycle 2 -60 Cycle 3 Cycle 4 Batteries 2022, 8, x FOR PEER REVIEW Figure 5. Cyclic voltammetric profiles of C-surgical (a) and of C-FFP2 (b) in 1 M NaClO4 in PC -90 Figure 5. Cyclic voltammetric profiles of C-surgical (a) and of C-FFP2 (b) in 1 M NaClO4 in PC recorded at a scan rate of 0.1 mV s−1 in t−h1e 0.05–3 V vs. Na+/Na ra+nge. recorded at a scan rate of 0.1 mV s in the 0.05–3 V vs. Na /Na range. corresponding Nyquist plots are shown in Figure 6). Both the fresh cells were 400 characterized by a very low intercept with the real axis (around 5 Ω), corresponding to a very low bulk resistance (Rb, mainly associated with the resistance of the electrolyte). The fresh cell 300 fresh semicircle amplitudaeftewr 3ahsreastssociated with the charge transfer resistance (Rafctet)r 3ohfreNst a+ ion after CV after CV diffusion between the electrode and the electrolyte. In contrast, the final straight line in 200 the low-fr6e0quency range was associated with a Warburg capacitance, associated with the diffusion 4o0f ions [49,50]. After 3 h, Rct increased for both samples (up to 100 Ω in the real 40 B (-Im(Z)/Ohm) Current density (mA cm-2g-1) B (-Im(Z)/Ohm) Current density (mA cm-2g-1) part for C-surgical), thus it was most likely associated with the interfacial layer growth 20 100 20 between the electrode and the electrolyte (SEI) [51]. Finally, after voltammetric cycling 00 0 20 40 60 80 100 120 140 0 20 40 60 80 100 120 140 (blue square spectra), the overall cell r0esistance decreased, most likely suggesting a 0 100 200 300 0 100 200 300 + stabilization of the SEI upon cycling, indicating a much easier diffusion of Na ions from Re(Z)/Ohm Re(Z)/Ohm the electrolyte to the electrode after a few electrically promoted cycles [50]. Figure 6. EIS spectra of C-surgical (a) and of C-FFP2 (b) in 1 M NaClO4 in PC vs. Na, recorded at Figure 6. EIS spectra of C-surgical (a) and of C-FFP2 (b) in 1 M NaClO4 in PC vs. Na, recorded at three different stages, i.e., just after assembling the cell, after 3 h of rest at OCV and after the cyclic three different stages, i.e., just after assembling the cell, after 3 h of rest at OCV and after the cyclic voltammetric analysis shown in Figure 5. voltammetric analysis shown in Figure 5. C-surgical and C-FFP2 showed similar behavior during galvanostatic cycling, as seen C-surgical and C-FFP2 showed similar behavior during galvanostatic cycling, as seen in Figure 7. Plots (a) and (d) highlight the charge/discharge profiles of C-surgical and C- in Figure 7. Plots (a) and (d) highlight the charge/discharge profiles of C-surgical and FFP2, respectively, in a Na-metal cell with the configuration Na/NaClO4/C at different C-FFP2, respectively, in a Na-metal cell with the configuration Na/NaClO4/C at different current regimes (C/20, C/10, C/5, C/2 and 1C) in the 0.05–3 V vs. Na+/Na r+ange. Typical current regimes (C/20, C/10, C/5, C/2 and 1C) in the 0.05–3 V vs. Na /Na range. Typical sloping profiles for hard carbon anodes upon reversible insertion/deinsertion of Na+ ions+ sloping profiles for hard carbon anodes upon reversible insertion/deinsertion of Na ions were observed. The specific capacity delivered by the cell exceeded 100 mAh g were observed. The specific capacity delivered by the cell exceeded 100 mAh g for surgical and 115 mAhg −1 −1 for C-FFP2 during the initial cycles at a C/20 rate. A capacity drop C-surgical and 115 mAhg for C-FFP2 during the initial cycles at a C/20 rate. A capacity occurred upon doubling the current rate to C/10, delivering 82 and 98 mAh g−1, −1 drop occurred upon doubling the current rate to C/10, delivering 82 and 98 mAh g , respectively. Further increases in the current rate caused a progressive decrease in the respectively. Further increases in the current rate caused a progressive decrease in the −1−1 −1−1 specifsicpeccaipfiaccictaypvaacliutyesv,awluheicsh,wheirceh6w4earned6840amndA8h0gmAathCg/5,4a3taCn/d55,843maAnhdg58amtACh/2g, at −1 −1 and 30C/an2,dan45dm30Aahndg45amt 1ACh. Ogveraatl1l,Ct.hOevoevrearlpl,ottheenotivaelripnoctrenatsiealwinhcirleaisnecrwehasiliengintchreaCsi-ngthe rate wCa-srartaethwearslirmatihtedr,liamccitoeudn,taicncgoufonrtitnhgefgoorotdheegleocotrdoenlieccctroondicuctoinvdituycotifvtihtyeocfotmhepocsoimteposite electroedleecst.rodes. 60 9 of 15 −1 −1 for C-PDF Image | From Wastes to Anode Materials for Na-Ion Batteries
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