Sulfide electrolyte materials, preparation method thereof and all-solid lithium secondary battery
A technology of sulfide electrolyte and electrolyte material, which is applied in the field of lithium-ion batteries, can solve the problems of low ion conductivity, achieve high ion conductivity, improve electrochemical stability, and improve compatibility
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[0046] The present invention also provides a preparation method of the sulfide electrolyte material represented by formula (I), comprising the following steps:
[0047] Will Li 2 S, P 2 S 5 with Li 3 PO 4 According to the molar ratio of 75:(25-x):x, after mixing, grinding, and then performing heat treatment, the sulfide electrolyte material shown in formula (I) is obtained;
[0048] 75Li 2 S·(25-x)P 2 S 5 ·xLi 3 PO 4 (I);
[0049] Among them, 0
[0050] In the process of preparing the sulfide electrolyte material shown in formula (I), the present invention is preferably carried out under a protective atmosphere, and Li 2 S, P 2 S 5 with Li 3 PO 4 Preferably, the mixture is mixed under the condition that the water content is less than 100ppm, and then ground and heat-treated to obtain the sulfide electrolyte material for an all-solid lithium secondary battery. The present invention has no special limitation on the mixing, and the raw materials can be mi...
Embodiment 1
[0071] Under the protection of argon atmosphere, Li with a purity of more than 99% 2 S, P 2 S 5 with Li 3 PO 4 After weighing according to the molar ratio of 75:24:1, manually grind and mix evenly under the condition that the water content is less than 100ppm, and then high-energy ball mill for 10 hours to obtain the primary powder material, take out the primary powder material and grind it evenly, and then use 10MPa pressure to press the tablet Get the flake raw material, put the flake raw material into the sintering mold, heat the sintering mold with the above flake raw material to 260°C at a heating rate of 2°C / min, keep it warm for 4h, and cool it to room temperature with the furnace. Under the condition that the water content is 0.1ppm, take out the sheet-shaped sintered product and grind it evenly to obtain a powder all-solid-state lithium secondary battery sulfide electrolyte material, that is, 75%Li 2 S 24%P 2 S 5 1% Li 3 PO 4 glass ceramics.
[0072]After obt...
Embodiment 2
[0078] Under the protection of argon atmosphere, Li with a purity of more than 99% 2 S and P 2 S 5 After weighing according to the molar ratio of 75:25, manually grind under the condition that the water content is less than 100ppm, and then use a high-energy ball mill for 7.5h to obtain 75%Li 2 S-25%P 2 S 5 Primary material of amorphous powder. at 75% Li 2 S-25%P 2 S 5 According to (75% Li 2 S-25%P 2 S 5 ): Li 3 PO 4 Add Li for a molar ratio of 80:20 3 PO 4 , and then continue ball milling for 15h to get 80% (75%Li 2 S·25%P 2 S 5 ) 20% Li 3 PO 4 Primary material of glass powder. Take out the above-mentioned glass powder primary material and grind it evenly, then use 10MPa pressure to press the tablet to obtain the flake primary material, put the flake primary material into the sintering mold, then put the sintering mold with the above-mentioned flaky primary material into the muffle furnace and Heat up to 260°C at a heating rate of 2°C / min, hold for 4 hours...
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