High-ion-conductivity sulfide solid electrolyte based on liquid phase method and preparation method thereof
A solid electrolyte, high-ion technology, applied in electrochemical generators, circuits, electrical components, etc., can solve problems such as the reduction of electrical conductivity, and achieve the effect of eliminating grain boundary resistance, improving electrolyte performance, and improving ionic conductivity.
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[0050] Example 1
[0051] In the glove box, weigh out Li according to 75∶25 2 S and P 2 S 5 , Added to the container containing dehydrated tetrahydrofuran. Stir at 600 rpm for 48h. The resulting suspension was vacuum filtered. The obtained powder was precipitated and dried at 150°C and -0.1MPa for 2h. Put the obtained powder into a sealed ball mill tank, vacuum the ball mill tank, and ball mill for 3 hours at a rotation speed of 300 rpm. Take out the material in the glove box, heat treatment at 200°C for 1 h under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.
[0052] The electrolyte obtained above was put into a mold, and hot pressed at 100 MPa and 100° C. for 30 minutes to obtain a sulfide solid electrolyte sheet with a thickness of 30 μm. The prepared solid electrolyte has an ionic conductivity of 1.3×10 at room temperature -3 S / cm.
Example Embodiment
[0053] Example 2
[0054] In the glove box, weigh Li according to 70:29 2 S, P 2 S 5 , Added to the container containing dehydrated tetrahydrofuran. Stir at 600 rpm for 24h. The resulting suspension was dried at 150°C and -0.1MPa for 12 hours. The obtained powder and the measurement ratio of P 2 O 5 (Li 2 S: P 2 S 5 : P 2 O 5 =70:29:1) Put it into a sealed ball mill jar, vacuum the ball mill jar, and ball mill for 3 hours at a speed of 300 rpm. Take out the material from the glove box and heat it at 230°C for 2h under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.
[0055] The electrolyte obtained above was put into a mold, and hot pressed at 100 MPa and 100° C. for 30 minutes to obtain a sulfide solid electrolyte sheet with a thickness of 30 μm. The prepared solid electrolyte has an ionic conductivity of 6.2×10 at room temperature -3 S / cm.
Example Embodiment
[0056] Example 3
[0057] In the glove box, weigh Li according to 70:25 2 S, P 2 S 5 , Added to a container containing anhydrous acetonitrile. Stir at 1000 rpm for 36 hours. The resulting suspension was dried at 150°C and -0.1MPa for 12 hours. The obtained powder and the metering ratio of LiCl (Li 2 S: P 2 S 5 :LiCl=70:25:5) Put it into a sealed ball mill jar, evacuate the ball mill jar, and ball mill for 3 hours at 300 rpm. Take out the material in the glove box, heat treatment at 260°C for 1 h under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.
[0058] Add the obtained electrolyte to the NMP sizing and apply it on the PET film, pass 5 sets of counter rolls (total length 0.6m) with a pitch of 30μm and a temperature of 150℃ at a speed of 10cm / min, and then peel off after vacuum drying at 80℃ for 1h. Sulfide electrolyte membrane. The prepared solid electrolyte has an ionic conductivity of 9.2×10 at room temperature -4 S / cm.
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