BATTERY DEMONSTRATION OF 3D ARCHITECTED CARBON ELECTRODES
3.5. Detailed Experimental Procedures Coin cell making process
The cells with 3D architected carbon electrodes were prepared using a stainless steel 2032 coin cell (20 mm diameter. 3.2 mm thickness, MTI). Half-cell was assembled against a lithium foil (99.9%, Sigma-Aldrich) as a counter and reference electrode with 1.0 M lithium hexafluorophosphate in 1:1 (v/v) ratio of ethylene carbonate: diethyl carbonate (Dongguan Shanshan Battery Materials) as received. In addition to standard parts of a coin cell (i.e. cases, electrodes, spring, separator, and spacer), a polypropylene washer was put surrounding the 3D architected carbon to make sure the carbon electrode was positioned in the projected region of the lithium foil. The polypropylene porous separator (gifted from Samsung) was used. The schematics of the components of the coin cell are illustrated in Figure 3. 1. The electrolyte was flooded in a coin cell, and coin cell assembly was conducted using a hydraulic
crimper (MTI) by applying 500 psi on the coin cell. All battery construction was performed in an Ar-filled glove box (HE-243-XW, Vacuum Atmospheres).
Galvanostatic cycling tests and electrode recycling
Galvanostatic cycling tests were conducted using the assembled coin cells by a battery testing machine (BTS3000, Neware) or a battery cycling system (BCS-805, Biologic) at room temperature. Open-circuit voltage was applied for more than four hours before starting cycling tests to obtain equilibrium. Slow current density cycling tests at 2 mA g-1 were performed to investigate discharge/charge behaviors without kinetics limitations. Step currents tests were also conducted at 16.7, 33.3, 66.7, 100, 200, 300 mA g-1 for every five cycles to evaluate the rate performance of the 3D architected carbon electrodes with different thicknesses. Open-circuit voltage was applied for ten hours before changing the current density. The step current tests were employed for a three-electrode configuration cell (PAT- Cell, EL-CELL) with 3D architected carbon with a 25.7 mg cm-2 mass loading as a working electrode, Li foil as a counter electrode, and another Li foil as a reference electrode with 1.0M lithium hexafluorophosphate in 1:1 (v/v) ratio of ethylene carbonate: diethyl carbonate.
The voltage between the working and reference electrode was monitored for cut-off voltages.
The voltage of the counter electrode against the reference electrode was also monitored.
For the 3D architected carbon, after step currents, 16.7 mA g-1 of the current density was applied for investigating the cycle life. Galvanostatic cycling tests at 100 mA g-1 were also conducted for more than 500 cycles following three pre-cycling at 16.7 mA g-1. For all galvanostatic cycling tests, cut-off voltages were set at 2 V and 0.005 V. After ending the charge process of the cycles at 100 mA g-1 for more than 300 cycles, the coin cell was disassembled with the caution not to deform the 3D architected carbon in the Ar-filled glove box. The cycled 3D architected carbon was rinsed, immersed in dimethyl carbonate (DMC) for overnight, and then dried for observation by SEM. The exposure of the carbon electrode to air while transferring the specimens was minimized up to a few seconds. The 3D architected carbon after 500 cycles was rinsed by DMC and then deionized water. The rinsed sample was dried in a vacuum oven overnight at over 100°C. The rinsing with DMC and
water and drying processes were repeated. Then, a new cell using the 3D architected carbon was assembled with a fresh electrolyte and tested by galvanostatic cycling at 100 mA g-1 following three pre-cycling at 16.7 mA g-1.
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