A kind of preparation method of diaphragm coating material with self-healing function
A coating material and self-repairing technology, applied in secondary battery repair/maintenance, structural parts, battery pack parts, etc. limited problems, to achieve the effect of improving electrochemical stability, improving electrochemical performance, and slowing down volume expansion
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Embodiment 1
[0026] 1) First weigh 1g of carbon nanotubes and measure 2ml of concentrated nitric acid with a mass fraction of 68wt% and 8ml of a mixed solvent of concentrated sulfuric acid with a mass fraction of 98wt% (1:4) in a three-necked flask. React for 12 hours, centrifuge and wash with deionized water continuously. After more than 20 times of centrifugal washing, put it into a vacuum drying oven for drying.
[0027] 2) Take 0.5 g of the acidified product from 1), disperse it in 100 ml of deionized water, and add 4 ml of 3-chloropropyltrimethoxysilane dropwise. Constant temperature oil bath, the temperature was controlled at 90°C, and reacted for 12 hours; after the reaction was completed, it was filtered, washed several times, put into a vacuum drying oven, and dried at 80°C for 12 hours.
[0028] 3) Take 0.96g of elemental sulfur and 2.4g of sodium sulfide nonahydrate in 50ml of deionized water, heat and stir for 3 hours to obtain a light yellow sodium polysulfide solution.
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Embodiment 2
[0034] 1) The difference from Example 1 is that after acidifying 1g of carbon nanotubes, it is dispersed in deionized water and added with 2g of cysteine hydrochloride (C 3 h 7 NO 2 S·HCl·H 2 O), continue to react at 70°C for 5h. In order to improve the grafting rate of sulfur, configure 30ml concentration of 3mol / L sodium polysulfide solution, where Na 2 The ratio of S:S was 1:1, and the remaining steps were the same as in Example 1, and finally cut into a diaphragm with a diameter of 19 mm.
[0035] 2) Prepare carbon-sulfur composite material (C:S=3:7), acetylene black AB, and LA133 in a ratio of 7:2:1 to prepare a positive electrode sheet with a diameter of 14mm, and use a metal lithium sheet as the negative electrode, and prepare it in step 1) The separator, electrolyte with 1M LiTFSI 2wt% LiNO 3 DOL:DME=1:1, make 2025 type button cells in the glove box.
Embodiment 3
[0037] 1) First take 1g of acetylene black and measure 5ml mass fraction of concentrated nitric acid of 68wt% and 15ml of mass fraction of 98wt% concentrated sulfuric acid mixed solvent (volume ratio 1:3) to be placed in a three-necked flask, through a constant temperature oil bath for 80 ℃ reaction for 12h, several times of centrifugation and washing, then placed in a vacuum oven to dry at 80℃ for 12h.
[0038]2) Take 0.5 g of the acidified product from 1), disperse it in 100 ml of deionized water, and add 2 ml of 3-chloropropyltrimethoxysilane dropwise. Constant temperature oil bath, the temperature was controlled at 90°C, and reacted for 12 hours; after the reaction was completed, it was filtered, washed several times, put into a vacuum drying oven, and dried at 80°C for 12 hours.
[0039] 3) Take 0.64g of elemental sulfur and 1.1g of anhydrous potassium sulfide in 20ml of deionized water, heat and stir for 3 hours to obtain a light yellow potassium polysulfide solution.
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