| Summary: | Li<sub>6</sub>PS<sub>5</sub>Cl possesses high ionic conductivity and excellent interfacial stability to electrodes and is known as a promising solid-state electrolyte material for all-solid-state batteries (ASSBs). However, the optimal annealing process of Li<sub>6</sub>PS<sub>5</sub>Cl has not been studied systematically. Here, a Box–Behnken design is used to investigate the interactions of the heating rate, annealing temperature, and duration of annealing process for Li<sub>6</sub>PS<sub>5</sub>Cl to optimize the ionic conductivity. The response surface methodology with regression analysis is employed for simulating the data obtained, and the optimized parameters are verified in practice. As a consequence, Li<sub>6</sub>PS<sub>5</sub>Cl delivers a rather high conductivity of 4.45 mS/cm at 25 °C, and ASSB consisting of a LiNi<sub>0.6</sub>Co<sub>0.2</sub>Mn<sub>0.2</sub>O<sub>2</sub> cathode and lithium anode shows a high initial discharge capacity of 151.7 mAh/g as well as excellent cycling performances for more than 350 cycles, highlighting the importance of the design of experiments.
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