Composite solid electrolyte and preparation method and application thereof
A solid electrolyte, quality technology, applied in the direction of non-aqueous electrolyte batteries, circuits, electrical components, etc., can solve the problems of cumbersome solid electrolyte production process, insufficient lithium ion conductivity, long cycle, etc., to reduce low interface impedance, Excellent discharge performance and short production cycle
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[0025] The invention proposes a method for preparing a composite solid electrolyte, which includes: mixing fluorine-containing polymers, lithium salts, nano-ceramic materials, organic alkali metal compounds, and organic solvents in a mass ratio of 100:1 to 200:1 to 100:0.001 to 10: 100-10000, perform high-energy dispersion treatment at a rate of 500-50000rpm, apply the slurry after high-energy dispersion treatment to form a film, and vacuum dry at 60-100°C for 12-72 hours to form a composite solid electrolyte.
[0026] Among them, the organoalkali metal compound is preferably organic alkali metal lithium; during the high-energy dispersion process, the C-F bond of the fluoropolymer is removed from the -F under the catalysis of the organoalkali metal lithium to form a localized double bond rich in π electrons Structured polymer and nano-lithium fluoride, in-situ modification of the surface layer of nano-ceramic materials by nano-lithium fluoride, and in-situ modification of nano-...
Embodiment 1
[0038] Add 675g of N-methylpyrrolidone and 25g of lithium bistrifluoromethanesulfonimide to a 1.5L stirring tank, mechanically stir at 500rpm for 15min, then slowly add 75g of polyvinylidene fluoride, and stir at room temperature for 12 hours at 1500rpm, Then add 5.2g nano-ceramic material Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 (LLZTO) Stirring was continued for 6 hours, resulting in a beige suspension. Then, 1ml of 10wt% lithium methoxide solution was added dropwise under stirring at 2000rpm, and finally a highly dispersed orange suspension, ie NMP suspension B of PVDF-LTFSI-LLZTO, was obtained. Take 7ml of the suspension with a syringe, and cast a coating film of 50cm in a glass disc 2 , 80 ℃ dynamic vacuum drying for 16 hours, punch out a diaphragm with a diameter of 16mm, test the AC impedance spectrum and calculate the lithium ion conductivity to be 3.0x10 -4 S / cm. It can be seen that the composite solid electrolyte has higher lithium ion conductivity.
Embodiment 2
[0040] Add 675g of N-methylpyrrolidone and 25g of lithium bistrifluoromethanesulfonimide into a 1.5L stirring tank, mechanically stir at 500rpm for 15min, then slowly add 75g of polyvinylidene fluoride, and stir at room temperature for 12 hours at 1500rpm, Then add 5.2g nano-ceramic material Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 (LLZTO) continued to stir for 6 hours to obtain a beige suspension, then added dropwise 2ml of 10wt% lithium methoxide solution under stirring at 2000rpm, and finally obtained a highly dispersed tan suspension, that is, the NMP suspension of PVDF-LTFSI-LLZTO c. Take 7ml of the suspension with a syringe, and cast a film of 50cm in a glass or PTFE disc 2 , 80°C dynamic vacuum drying for 16 hours, punch out a diaphragm with a diameter of 16mm, test the AC impedance spectrum and calculate the lithium ion conductivity to be 2.6x10 -4 S / cm.
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