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Dry preparation process of solid electrolyte

A technology for solid electrolyte and preparation process, applied in the field of dry preparation process of solid electrolyte, can solve the problems of volatilization and loss of lithium, and achieve the effects of reducing volatilization of lithium, avoiding pollution and harm, and high density

Active Publication Date: 2022-01-04
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, wet ball milling is adopted, and secondary sintering is carried out by embedding powder at 950-1150°C for 15-24 hours, which easily leads to volatilization and loss of lithium.

Method used

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  • Dry preparation process of solid electrolyte
  • Dry preparation process of solid electrolyte
  • Dry preparation process of solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]Weigh lithium hydroxide, lanthanum oxide, zirconium oxide, and tantalum oxide sequentially according to the mass fractions of 15%, 50%, 20%, and 15%, respectively, using zirconia balls and polyurethane ball milling tanks, and dry method at a speed of 175r / min Ball mill for 2 hours, then use a sieve to separate the balls and powder. Transfer the powder to an alumina crucible for pre-sintering. The sintering system is 5°C / min and the temperature is raised to 950°C. After 3 hours of heat preservation, it is cooled to room temperature with the furnace, and the secondary dry ball milling is performed at a speed of 175r / min. Zirconium balls and polyurethane ball milling tank, the ball milling time is 2 hours, after ball milling, the ball material is separated to obtain master powder. Weigh 1 g of mother powder, hold the pressure at 500 MPa for 1 min to obtain a green body, the diameter of the green body is 12 mm. The ceramic green body was transferred to a magnesia crucible w...

Embodiment 2

[0040] Weigh lithium hydroxide, lanthanum oxide, zirconium oxide, and tantalum oxide sequentially according to the mass fractions of 30%, 45%, 15%, and 10%, respectively, using zirconia balls and polyurethane ball milling jars, and dry method at a speed of 300r / min Ball milling was carried out for 0.5 hour, after which the balls and powder were separated using a screen. Transfer the powder to an alumina crucible for pre-sintering. The sintering system is 5°C / min and the temperature is raised to 900°C. After 3 hours of heat preservation, it is cooled to room temperature with the furnace, and the secondary dry ball milling is performed at a speed of 300r / min. Zirconium balls and polyurethane ball milling tank, the ball milling time is 0.5 hours, after ball milling, the ball material is separated to obtain the mother powder. Weigh 0.5g of mother powder, hold the pressure at 100MPa for 1min to obtain a green body, the diameter of the green body is 12mm. The ceramic green body was...

Embodiment 3

[0043] Weigh lithium hydroxide, lanthanum oxide, zirconium oxide, and tantalum oxide sequentially according to the mass fractions of 15%, 50%, 20%, and 15%, using tungsten carbide balls and nylon ball mill jars, and dry method at a speed of 250r / min Ball mill for 2.5 hours, then use a screen to separate the balls and powder. Transfer the powder to an alumina crucible for pre-sintering. The sintering system is 5°C / min to 850°C. After 6 hours of heat preservation, it is cooled to room temperature with the furnace. The secondary dry ball milling is carried out at a speed of 175r / min. Tungsten ball and nylon ball milling tank, the ball milling time is 2 hours, after ball milling, the ball material is separated to obtain the mother powder. Weigh 2g of mother powder, hold the pressure at 1000MPa for 1min to obtain green body, the diameter of green body is 12mm. The ceramic green body was transferred to a magnesia crucible with an inner diameter of 15mm, and the secondary sintering ...

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Abstract

The invention relates to a lithium battery electrolyte, and especially relates to a dry preparation process of a solid electrolyte. The dry preparation process comprises the following steps: mixing lanthanum oxide, zirconium oxide, a lithium source and a doping raw material, and uniformly grinding to obtain a mixture; presintering the mixture, and cooling to room temperature; carrying out secondary grinding on the pre-sintered mixture to obtain mother powder; tabletting the mother powder to obtain a biscuit; and carrying out secondary sintering on the biscuit to obtain the solid electrolyte. Compared with the prior art, the process has the advantages that the magnesium oxide crucible is adopted for secondary sintering, and short-time sintering is carried out at high temperature, so that the volatilization of lithium in the high-temperature process can be effectively reduced, and the formation of secondary phases such as lanthanum zirconate and the like is avoided. The LLZO prepared by the process has the characteristics of higher density, almost no grain boundary and the like, and almost no lithium oxide is enriched at the grain boundary, so that the LLZO prepared by the process has higher air stability.

Description

technical field [0001] The invention relates to a lithium battery electrolyte, in particular to a dry preparation process of a solid electrolyte. Background technique [0002] Commercial lithium-ion batteries have potential safety hazards due to the use of liquid electrolytes containing flammable organic solvents. The development of all-solid-state lithium batteries is one of the feasible technical approaches to improve battery safety. Among various solid electrolyte materials, garnet-type solid electrolytes are preferred due to their advantages of non-flammability, high safety, good chemical and electrochemical stability, lithium ion migration number close to 1, and high room temperature conductivity. attention. [0003] Since 2003, Thangadurai et al. synthesized lithium-containing garnet (hereinafter referred to as LLZO) for the first time using solid-state sintering method, and many scientific researchers began to invest in the research of LLZO. LLZO is a fast conducto...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/50C04B35/48C04B35/622H01M10/0525H01M10/0562H01M10/058
CPCC04B35/50C04B35/48C04B35/622H01M10/0562H01M10/058H01M10/0525H01M2300/0071C04B2235/3227C04B2235/3203C04B2235/442C04B2235/3217C04B2235/3251C04B2235/3286C04B2235/6562C04B2235/6567C04B2235/77C04B2235/96Y02E60/10Y02P70/50
Inventor 段华南郑鸿鹏李国耀黄晓欧阳诚吴勇民
Owner SHANGHAI JIAO TONG UNIV
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