US 12,278,334 B2
Lithium-aluminum hydrotalcite-based solid electrolyte film working at room temperature, preparation method thereof, and lithium battery including same
Wen Liu, Beijing (CN); Minggui Xu, Beijing (CN); Xiaoming Sun, Beijing (CN); Jijin Yang, Beijing (CN); Ting Gao, Beijing (CN); and Xiwen Lu, Beijing (CN)
Assigned to Beijing University of Chemical Technology, Beijing (CN)
Appl. No. 18/696,871
Filed by BEIJING UNIVERSITY OF CHEMICAL TECHNOLOGY, Beijing (CN)
PCT Filed Dec. 22, 2021, PCT No. PCT/CN2021/140302
§ 371(c)(1), (2) Date Mar. 28, 2024,
PCT Pub. No. WO2023/082434, PCT Pub. Date May 19, 2023.
Claims priority of application No. 202111337243.0 (CN), filed on Nov. 12, 2021.
Prior Publication US 2024/0421347 A1, Dec. 19, 2024
Int. Cl. H01M 10/0562 (2010.01); H01M 10/0525 (2010.01)
CPC H01M 10/0562 (2013.01) [H01M 10/0525 (2013.01); H01M 2300/0068 (2013.01)] 5 Claims
OG exemplary drawing
 
1. A method for preparing a lithium aluminum hydrotalcite-based solid electrolyte film working at room temperature, comprising:
step 1) dissolving a water-soluble lithium salt, a water-soluble aluminum salt, and a water-soluble meta-aluminate in deionized water that has been introduced with an inert gas and boiled to remove carbon dioxide, subjecting a resulting mixture to ultrasound or stirring to dissolve, then adding an alkali thereto to adjust a pH of the resulting mixture to 9 to 11, and controlling a temperature at 60° C. to 80° C., and subjecting a resulting adjusted mixture to reaction to produce a lithium aluminum hydrotalcite;
step 2) placing the lithium aluminum hydrotalcite obtained in step 1) under protection of an inert gas, calcining at 100° C. to 150° C. for 2 h to 6 h to remove water between hydrotalcite layers to obtain a calcined sample, then grinding the calcined sample to power to obtain a lithium aluminum hydrotalcite powder;
step 3) preparing a lithium aluminum hydrotalcite-based solid electrolyte slurry for later use by the following operations in a first glove box:
adding an organic solvent, an organic polymer, and a lithium salt into a container, stirring an obtained mixture to complete dissolution, then adding the lithium aluminum hydrotalcite powder to the obtained mixture, subjecting a resulting blend to ultrasound or stirring to homogeneous dispersion, then adding a photoinitiator or a thermal initiator thereto to obtain the lithium aluminum hydrotalcite-based solid electrolyte slurry; and
wherein the organic polymer is polyethylene glycol diacrylate (PEGDA); and
step 4) performing the following operations in a second glove box:
subjecting the lithium aluminum hydrotalcite-based solid electrolyte slurry obtained in step 3) to curing and film-forming to obtain the lithium aluminum hydrotalcite-based solid electrolyte film;
wherein proportions of an inorganic phase and an organic phase in the solid electrolyte film are respectively as follows: a content of an inorganic phase lithium aluminum hydrotalcite is 59.9 wt %, and a content of the organic phase is 40.1%, based on a total mass of a solid electrolyte film after removal of the lithium salt; and
in step 1), the water-soluble lithium salt is lithium chloride; the water-soluble aluminum salt is aluminum chloride; and a molar ratio of lithium to aluminum is in a range of 1:2 to 1:5.