Preparation method of sulfide solid electrolyte
A solid electrolyte and sulfide technology, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve the problems of high price, low purity of lithium sulfide, and difficulty in industrialized production, and achieve the effect of low price and easy industrialization.
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Embodiment 1
[0023] Dry the raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate in a vacuum drying oven at 100°C for 12h. Under the protection of argon atmosphere, 2.24g of sulfur powder, 1.12g of lithium hydride, 6.66g of phosphorus pentasulfide and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill jar. The mass ratio is 20:1, and the ball is milled for 60h under the condition of 400r / min at room temperature. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace in a nitrogen atmosphere of 80 mL / min. The sintering temperature was 300 °C, and the sintering time was 4h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.
Embodiment 2
[0025] Dry the raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate in a vacuum drying oven at 80°C for 18h. Under the protection of argon atmosphere, 2.56g of sulfur powder, 1.28g of lithium hydride, 4.44g of phosphorus pentasulfide and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill jar. The mass ratio is 30:1, and the ball is milled at room temperature for 48h under the condition of 500r / min. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace under a nitrogen atmosphere of 40 mL / min. The sintering temperature was 260 °C, and the sintering time was 3h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.
Embodiment 3
[0027] The raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate were dried in a vacuum drying oven at 60°C for 24h. Under the protection of argon atmosphere, 2.4g of sulfur powder, 1.2g of lithium hydride, 5.55g of phosphorus pentasulfide, and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill. The mass ratio is 40:1, and the ball is milled for 36h under the condition of 300r / min at room temperature. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace under a nitrogen atmosphere of 60 mL / min. The sintering temperature was 280 °C, and the sintering time was 5h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.
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