From Wastes to Anode Materials for Na-Ion Batteries

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From Wastes to Anode Materials for Na-Ion Batteries ( from-wastes-anode-materials-na-ion-batteries )

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Batteries 2022, 8, 183 4 of 13 adsorption at −196 ◦C on a micrometrics Tristar II instrument (Micromeritics Instrument Corporation, Norcross, GA, USA). The Brunauer–Emmett–Teller (BET) model was applied to analyze the data. 2.3. Na-Metal and Na-Ion Cell Assembly and Electrochemical Testing In this work, both lab-scale Na-metal cells and Na-ion cells were assembled and tested. Na-metal cells were assembled using a Whatman GF/A glass wool disk soaked with 200 μL of electrolyte (NaClO4 1 M in propylene carbonate, Solvionic, Toulouse, France) as the separator. After assembly, the cells were left 4 h at OCV, waiting for equilibration before testing. They were cycled between 0.05 V and 3 V vs. Na+/Na. The pyrolyzed FM powder was used as the active material (mass loading of ca. 1.5 mg/cm2 for both C-surgical and C-FFP2) and Na metal was used as both the counter and reference electrodes. Na-ion cells assembled using a Whatman GF/A glass wool disk as the separator, soaked with 200 μL of electrolyte (NaClO4 1 M in propylene carbonate, Solvionic). Na3V2(PO4)2F3 (NVPF), prepared from NH4H2PO4, V2O5 and NaF precursors heated under an Ar atmosphere at 650 ◦C [35], was used as cathode (mass loading of 2.0 mg/cm2). The Na-ion cell was galvanostatically cycled at 0.1 mA/cm2 in the 1–4.1 V potential range vs. Na+/Na. Both cells were galvanostatically cycled at ambient laboratory temperature using an ARBIN BT2000 battery tester. The cells were cycled at different current rates, where the rate denoted as C/n corresponds to a full discharge (or a full charge) in n hours, based on an envisaged theoretical capacity (C) of 350 mAhg−1 for the Na/HC cells and 100 mAhg−1 for the HC/NVPF full cells. Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) were performed using a VMP3 electrochemical workstation from BioLogic Science Instruments (Seyssinet-Pariset, France). EIS measurements were performed at the open circuit potential (OCV) with an oscillating potential of 10 mV in the 300 kHz–0.1 Hz frequency range. CV was performed in the range of 0.05 and 3 V vs. Na+/Na with a scan rate of 0.1 mV s−1. Electrochemical tests were performed using ECC-Std test cells (EL-Cell GmbH, Hamburg, Germany). The test cells were assembled inside the Ar-filled glove box to avoid moisture contamination and left for 4 h at OCV before running the measurements. 3. Results Batteries 2022, 8, x FOR PEER REVIEW 5 of 15 The FMs were preliminarily characterized by means of IR spectroscopy in the ATR 3.1. Materials Characterization mode. The resulting spectra are shown in Figure 1. ν(CH2)a surgical FFP2 ν(CH3)s ν(CH2)s ν(CH) 2900 2800 2500 ν(CH3)a δ(CH3)a δ(CH3)s δ(CH2) δ(CH) Absorbance (a.u.) 3000 1450 1350 1000 950 3500 3000 2000 1500 1000 Wavenumbers (cm-1) Figure 1. FT-IR (ATR mode) of surgical and FFP2 FMs in the range from 500 to 3500 cm−1.−1 Figure 1. FT-IR (ATR mode) of surgical and FFP2 FMs in the range from 500 to 3500 cm . Accordingly to Fadare et al. [2], both surgical and FFP2 face masks are mainly composed of fibers of polypropylene (PP). Indeed, both spectra showed the characteristic features of PP, such as the asymmetric and symmetric ν(CH3) at 2950 and 2868 cm−1 (with shoulders at 2959 and 2877 cm−1 because of different phase resonance among neighboring units), the asymmetric and symmetric ν(CH2) at 2918 cm−1 and 2838 cm−1, the asymmetric and symmetric δ(CH3) at 1456 cm−1 and 1375 cm−1, δ(CH2) at 1437 cm−1 and δ(CH) at 1359

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