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electrolyte (posolyte and negolyte) was 50 mL of 1.0 M FeCl2 / 1.0 M CrCl3 in 3.0 M HCl. Humidified nitrogen gas (Airgas, 99.999%) was bubbled through the electrolytes for > 1 h to purge residual oxygen prior to the electrochemical measurements. A flow rate of ca. 93 mL min-1 was maintained with a MasterFlexTM pump set at 100 rpm and circulated using LS/16 NorpreneTM tubing (Cole-Parmer). The cell temperature was maintained at ca. 50 ± 5 °C using silicone adhesive-mount heating pads with a 10 W in–2 heating density (McMaster-Carr) connected to a benchtop PID controller (Platinum Series, CS8DPT, OMEGA Engineering), calibrated to the internal temperature of the cell components using a thermocouple probe (McMaster-Carr). The cell was cycled at a constant current density of 50 mA cm-2 between upper and lower cell voltage cutoffs of 1.2 V and 0.8 V, respectively, using an Arbin battery tester (FBTS-8). Purification Protocol – To purify the negative electrolyte, the subscale cell was charged starting from 0% state-of-charge (SOC) at 50 °C at 100 mA cm–2 until a cutoff voltage of 1.5 V was reached. A potential beyond the cycling voltage cutoff of 1.2 V was set to favorably drive cathodic plating reactions on the negative electrode, thus maximizing reduction of contaminants out of solution and onto the electrode without over-oxidizing the positive electrode. Following the galvanostatic precharge, the electrolytes were recirculated into their respective reservoirs, the cell was disassembled, the used electrodes on both sides were removed and fresh electrodes were inserted into the cell. To avoid air ingress and self-discharge, the reservoirs remained sealed throughout the entire process of replacing the electrode. The purified electrolyte was subsequently discharged in the reassembled cell, thus initiating the cycling protocol. Scanning Electron Microscopy (SEM) / Energy Dispersive X-ray Spectroscopy (EDS) – SEM was performed using a Zeiss Merlin High-Resolution SEM. A 10 keV electron energy and 9.2 mm working distance with an in-lens secondary electron detector were used. Using the same acquisition parameters, energy dispersive spectroscopy (EDS) was used for elemental mapping of post-purified electrodes. 93PDF Image | Bringing Redox Flow Batteries to the Grid
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