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2. Methods Cyclic voltammetry in elevated temperature – Ex situ electrochemistry was conducted in a three- electrode cell with a 3-mm diameter glassy carbon electrode (BASi), Pt coil (BASi), and Ag/AgCl in a 3 M NaCl reference electrode (BASi). The glassy carbon electrode was mirror-polished in a 0.05 μm MicroPolish alumina powder (Buehler) slurry on a microcloth disk, briefly sonicated in acetone and deionized (DI) water, rinsed in DI water, and allowed to air-dry. Chromium (III) chloride hexahydrate (CrCl3•6H2O, ≥99.5%, Alfa Aesar, Lot No. Q16G036), iron (II) chloride tetrahydrate (FeCl2•4H2O, 98%, Alfa Aesar, Lot No. S18H053), and hydrochloric acid (HCl, 37%, balance of water, Sigma Aldrich) were dissolved in DI water (Milli-Q Millipore, 18.2 MΩ cm). The electrolyte was 1.0 M FeCl2 / 1.0 M CrCl3 in 3.0 M HCl. A temperature of ca. 50 ± 5 °C was maintained by submerging a sealed vessel containing the electrodes and electrolyte into an oil bath heated by a VWR® Professional Hot Plate Stirrer with a temperature probe (VWR). Cyclic voltammograms were measured at a scan rate of 50 mV s–1, starting from open circuit potential, scanning in the positive direction to a voltage bound of 1.2 V vs Ag/AgCl, scanning in the negative direction to -1.0 V vs Ag/AgCl, and returning to the starting potential. Full iR-correction (100%) was employed during data acquisition by a Bio-Logic VSP potentiostat (Bio-Logic). Heat-treatment of electrodes – Sigracet (SGL) 39AA (Fuel Cell Store) electrodes were thermally oxidized in a muffle furnace (Barnstead Thermolyne Type 47900), ramping at a rate of 20 °C min- 1 from room temperature to 500 °C, holding for 5 h, and cooling down to ambient conditions without further intervention. The electrodes were subsequently stored under air in plastic containers (McMaster-Carr). Full cell RFB operation – Single-cell RFB cycling was performed in a subscale cell with a 5 cm × 5 cm (25 cm2) active electrode area. 3× thermally-treated SGL 39AA were used for both positive and negative electrodes. The thickness of PTFE gaskets were selected such that the electrode stack was compressed by ca. 20%. Interdigitated flow fields, milled from Tokai G347B resin- impregnated graphite plates of 3.18 mm thickness (Tokai Carbon Co.), were also employed, along with a NafionTM 117 membrane presoaked in 3.0 M HCl for ≥ 24 h. The starting solution for each 92PDF Image | Bringing Redox Flow Batteries to the Grid
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