All-solid-state batteries employing inorganic solid electrolytes are considered a promising next-generation energy storage system. Especially, argyrodite-type Li 6 PS 5 Cl (LPSCl) was highlighted for its good ionic conductivity and malleability. In the electrode level, achieving an efficient Li + pathway even with the maximized active material proportion and electrode mass loading is vital for a high energy density. Therefore, a smaller solid electrolyte particle is highly sought for. Herein, we demonstrated a spiral jet mill process for refining LPSCl particle size. The mean particle size (D 50 ) of LPSCl was reduced from 39.9 to 1.9 μm where the ionic conductivity was decreased from 2.0 to 0.23 mS cm −1 . The postannealing in a mild-temperature range (T < 250 °C) led to the even more decreased ionic conductivity. Although the ionic conductivity was restored when T > 300 °C, this high-temperature annealing resulted in severe particle agglomeration. Spectroscopic observations revealed that particle surfaces were damaged during pulverization and irreversible sulfur losses occurred during the mild-temperature annealing.
To mitigate poor contact issues between electrolyte/electrode materials interfaces of all‐solid‐state batteries (ASSB), we newly introduce a novel solution‐processed synthesis that exploits the differences in the boiling point and polarity of the two solvents (i. e., methanol, and toluene), with a cavitation effect by bubbling inert gas. Through this process, called solvent exchange with bubbles (SEB), the Li6PS5Cl solid electrolyte is synthesized with a particle size below 800 nm and sufficient ionic conductivity of 1.54 mS/cm at 25 °C. In addition, the ASSB cell consisting of the cathode electrode with Li6PS5Cl synthesized by the SEB exhibited a high capacity of 176 mAh/g at 0.1 C (55 °C) owing to the improved contact between the electrode and solid electrolyte. In particular, the rate capability of the cell is superior to that of a cell with Li6PS5Cl prepared by ball milling.
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