| CPC H01M 10/056 (2013.01) [C01B 21/0761 (2013.01); C01B 21/0768 (2013.01); C08J 3/2053 (2013.01); C08K 5/43 (2013.01); C08K 7/04 (2013.01); D01F 9/08 (2013.01); D01F 11/00 (2013.01); D04H 1/4209 (2013.01); D04H 1/4282 (2013.01); D04H 1/728 (2013.01); D06C 7/00 (2013.01); H01M 10/0525 (2013.01); C08J 2327/18 (2013.01); C08J 2327/20 (2013.01); C08K 2201/001 (2013.01); D10B 2101/14 (2013.01); D10B 2505/00 (2013.01); H01M 2300/0017 (2013.01); H01M 2300/0085 (2013.01)] | 4 Claims |
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1. A preparation method of a titanium nitride fiber-enhanced quasi-solid-state electrolyte, comprising the following steps:
I. preparation of TiN nanofiber:
1 adding polyvinylpyrrolidone to a mixed solution of anhydrous ethanol and glacial acetic acid and magnetically stirring to dissolution of polyvinylpyrrolidone, and then adding tetrabutyl titanate and continuing stirring to form a uniform solution, so as to obtain an electrospinning precursor solution;
wherein in the step I 1, a volume ratio of anhydrous ethanol to glacial acetic acid in the mixed solution of anhydrous ethanol and glacial acetic acid in the step I M is 7:3;
in the step I 1, a ratio of a mass of polyvinylpyrrolidone to a volume of the mixed solution of anhydrous ethanol and glacial acetic acid is (1 g to 2 g):10 mL;
in the step I M, a volume ratio of tetrabutyl titanate to the mixed solution of anhydrous ethanol and glacial acetic acid is (2 mL to 4 mL): 10 mL,
2 loading the electrospinning precursor solution into a syringe and then mounting the syringe inside an electrospinning machine, and then performing electrospinning to obtain a fiber felt;
wherein in the step I 2, the electrospinning uses No. 22 needle, a liquid supply rate is 1 mLh−1 to 2 mLh−1, a voltage is 15 kV to 30 kV, and a distance between the needle and an electrode olate is 15 cm to 20 cm;
3 heating the fiber felt to a calcination temperature in an air atmosphere and then calcining at the calcination temperature to obtain TiO2 nanofiber;
wherein in the step I 3, a rate of the heating is 1° C. min−1 to 3° C. min−1; and
in the step I 3, the calcination temperature is 500° C. to 550° C.; and a time of the calcination is 2 h to 4 h;
4 placing the TiO2 nanofiber into a tubular furnace and then introducing a mixed gas of NH3 and Ar into the tubular furnace, and heating the tubular furnace to the calcination temperature and then calcining at the calcination temperature to obtain TiN nanofiber;
wherein in the step I 4, a volume ratio of NH3 to Ar in the mixed gas of NH3 and Ar is 1:1, and a flow rate of NH3 is 80 sccm to 100 sccm;
in the step I 4, a rate of the heating is 50° C. min−1 to 10° C. min−1;
in the step I 4, the calcination temperature is 900° C. to 1000° C.; and
in the step I 4, a time of the calcination is 1.5 h to 3 h;
II. preparation of electrolyte:
1 adding the TiN nanofiber to N,N-dimethylformamide for ultrasonic treatment and then adding PVDF-HFP and LiTFSI and magnetically stirring to obtain a casting solution;
wherein in the step II 1, a mass ratio of the TiN nanofiber to PVDF-HFP to LiTFSI is (1 to 5):(50 to 75):(20 to 45);
in the step II 1, a mass fraction of the TiN nanofiber in the casting solution is 0.2% to 1%;
2 performing vacuum defoaming on the casting solution and then casting the casting solution on a glass plate, and then scraping into a film by using a scraper, and finally drying to obtain the titanium nitride fiber-enhanced quasi-solid-state electrolyte.
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