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All-solid-state lithium ion electrolyte material and preparation method thereof

An electrolyte material, lithium ion technology, applied in chemical instruments and methods, circuits, electrical components, etc., can solve the limited improvement of grain boundary conductivity and total conductivity, the conductivity of electrolyte materials needs to be improved, and molten salt is mixed into powder. Body and other problems, to achieve the effect of excellent electrochemical performance, low cost, and improved conductivity

Inactive Publication Date: 2019-05-07
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The whole process steps take too long, and the conductivity of the final electrolyte material needs to be improved
Chinese patent publication number CN103496740A has reported a kind of molten salt method to prepare Li 7 La 3 Zr 2 o 12 The method of electrolyte powder, which uses KCl and LiCl as molten salt, although the sintering temperature can be appropriately reduced, but the molten salt is easily mixed into the powder after sintering, which is difficult to wash off, resulting in low product purity
In this method, amorphous silicon oxide is used to improve the grain boundary conductivity of LLTO, but the added nano-silicon oxide layer is a lithium ion insulator, which has a limited effect on improving the grain boundary conductivity and total conductivity.
[0006] At present, it is basically the research on the above LLZO solid electrolyte and LLTO solid electrolyte materials, all of which have disadvantages such as poor electrochemical performance and low product purity.
In the prior art, there is no relevant report on the new type of electrolyte material-fast ion conductor lithium titanium aluminum phosphate

Method used

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  • All-solid-state lithium ion electrolyte material and preparation method thereof
  • All-solid-state lithium ion electrolyte material and preparation method thereof
  • All-solid-state lithium ion electrolyte material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Using lithium nitrate, aluminum nitrate, n-butyl titanate and phosphoric acid as raw materials, according to Li 1+x al x Ti 2-x (PO 4 ) 3 (Where x = 0.1, 0.2, 0.3, 0.4, 1, 1.1) stoichiometric ratio in the aqueous solution of ethanol, then add acetylacetone (according to 2 times the theoretical amount added), hydrolysis 8h under stirring at 60 ° C to obtain a uniform The solution, sol or suspension is then spray-dried, the inlet air temperature is 150°C, the outlet air temperature is 100°C, the feed rate of the peristaltic pump is 1000mL / h, and finally the obtained product material is kept at 800°C for 8 hours in an air atmosphere , that is, the walnut-shaped fast ion conductor material Li 1+x al x Ti 2-x (PO 4 ) 3 , the resulting product was pressed into tablets under certain pressure conditions to prepare an all-solid electrolyte, and then assembled with a lithium cobaltate positive electrode and a lithium metal negative electrode to form a button battery. The ...

Embodiment 2

[0034] Using lithium oxalate, aluminum oxalate, n-butyl titanate and ammonium dihydrogen phosphate as raw materials, according to Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 The stoichiometric ratio is mixed in an aqueous solution of ethanol, then acetylacetone is added (according to 2 times the theoretical amount), hydrolyzed for 8 hours under vigorous stirring at 60°C to obtain a uniform solution, sol or suspension, and then spray-dried. The air temperature is 150°C, the outlet air temperature is 100°C, and the feed rate of the peristaltic pump is 1000mL / h. Finally, the obtained product materials are kept at 500, 600, 700, 800, 1000, 1200, and 1300°C for 8 hours in an air atmosphere. The walnut-shaped fast ion conductor material Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 , the resulting product was pressed into tablets under certain pressure conditions to prepare an all-solid electrolyte, and then assembled with a lithium cobaltate positive electrode and a lithium metal negative electrode to...

Embodiment 3

[0039] Using lithium oxalate, aluminum oxalate, n-butyl titanate and ammonium dihydrogen phosphate as raw materials, according to Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 The stoichiometric ratio is mixed in an aqueous solution of ethanol, then acetylacetone is added (according to 2 times the theoretical amount), hydrolyzed for 8 hours under vigorous stirring at 60°C to obtain a uniform solution, sol or suspension, and then spray-dried. The air temperature is 150°C, the outlet air temperature is 100°C, and the feed rate of the peristaltic pump is 1000mL / h. Finally, the obtained product material is kept at 800°C in an air atmosphere for 1, 2, 4, 6, 8, 10, and 11 hours respectively. The walnut-shaped fast ion conductor material Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 , the resulting product was pressed into tablets under certain pressure conditions to prepare an all-solid electrolyte, and then assembled with a lithium cobaltate positive electrode and a lithium metal negative electrode to f...

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Abstract

The invention provides an all-solid-state lithium ion electrolyte material and a preparation method thereof. The method specifically comprises the following steps: (1) adding a lithium source, an aluminum source, a titanium source and a phosphorus source into a water solution of ethanol according to a stoichiometric ratio of Li<1+x>Al<x>Ti<2-x>(PO4)3, wherein x is greater than 0 and less than or equal to 1, then adding a complexing agent, and carrying out hydrolyzing to obtain a uniform solution, sol or turbid liquid; (2) carrying out spray drying on the solution, sol or turbid liquid obtainedin the step (1); and (3) heating the product obtained in the step (2) to 600-1200 DEG C in an air atmosphere, carrying out temperature-control calcinations for 2-10 hours, and then carrying out natural cooling to obtain the walnut-like fast-ion conductor material titanium aluminum lithium phosphate. The all-solid-state lithium ion electrolyte material prepared by the preparation method is in a special morphology, is distributed in a monodisperse manner and has relatively high room-temperature ionic conductivity and excellent rate and cycle performance; and no other impurity elements are introduced, so that the product purity is high.

Description

technical field [0001] The invention relates to the field of lithium ion battery materials and preparation methods thereof, in particular to an all-solid lithium ion electrolyte material and preparation methods thereof. Background technique [0002] Lithium-ion batteries have been invented since the 1990s, and their popularity has grown rapidly. However, traditional commercial lithium-ion batteries are mainly lithium-ion batteries assembled with organic electrolytes. The non-aqueous system of electrolyte lithium salts and the physical and chemical properties of the metal shell make lithium-ion batteries prone to fires under long-term use and high temperature conditions. A series of safety hazards such as electrolyte leakage, short circuit and explosion, and the electrolyte will react severely with the electrode interface when the battery is working, resulting in poor cycle and rate performance of the battery. Therefore, if the battery does not contain or contains a small amo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M10/0562H01M10/0525
CPCY02E60/10
Inventor 肖围王脂胭缪畅寇芝艳田明磊梅平
Owner YANGTZE UNIVERSITY
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