Preparation method of sulfide solid electrolyte

A technology of solid electrolyte and sulfide, applied in circuits, electrical components, secondary batteries, etc., can solve the problems of long time consumption and uneven mixing, and achieve the effects of high conductivity, good contact reaction, and shortened reaction time

Pending Publication Date: 2022-07-05
SHANGHAI FIRM-LITHIUM NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to provide a liquid-phase method for preparing argentite-type sulfide solid electrolytes. This method prepares solid-state electrolytes through solution methods, which solves the problems of long time-consuming and uneven mixing of traditional methods, and to a certain extent Increased conductivity, can reach 7mS cm -1

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  • Preparation method of sulfide solid electrolyte
  • Preparation method of sulfide solid electrolyte

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Embodiment 1

[0046] This embodiment provides a sulfide solid state electrolyte Li 6 PS 5 The preparation method of Cl, concrete steps are as follows:

[0047] (1) In the glove box, under the argon atmosphere, weigh Li according to the molar ratio of 3:1 2 S and P 2 S 5 , fully ground in an agate mortar, and uniformly ultrasonically dispersed in ultra-dry tetrahydrofuran, the ultrasonic time is 10min, and the frequency is 25kHz.

[0048] (2) The mixture obtained in step (1) was stirred at room temperature overnight for 10 h under the protective conditions of anhydrous and oxygen-free to obtain Li with a mass fraction of 1% 3 PS 4 • 3THF / THF suspension.

[0049] (3) In a glove box filled with argon gas, weigh Li according to the molar ratio of 1:1 2 S and LiCl were dissolved in anhydrous acetone to prepare a solution with a mass fraction of 3%.

[0050] (4) adding the solution obtained in step (3) to the suspension obtained in (2) in a volume ratio of 1:1. The suspension was stirred...

Embodiment 2

[0056] This embodiment provides a sulfide solid state electrolyte Li 6 PS 5 The preparation method of Br, the concrete steps are as follows:

[0057] (1) In the glove box, weigh Li at a molar ratio of 3:1 under an argon atmosphere. 2 S and P 2 S 5 , fully ground in an agate mortar, and uniformly ultrasonically dispersed in ultra-dry tetrahydrofuran, the ultrasonic time is 10min, and the frequency is 25kHz.

[0058] (2) The mixture obtained in step (1) was stirred at room temperature overnight for 10 h under the protective conditions of anhydrous and oxygen-free to obtain Li with a mass fraction of 1% 3 PS 4 • 3THF / THF suspension.

[0059] (3) In a glove box filled with argon gas, weigh Li according to the molar ratio of 1:1 2 S and LiBr were dissolved in anhydrous acetone to prepare a solution with a mass fraction of 4.2%.

[0060] (4) The solution obtained in step (3) is added to the suspension obtained in (2). The volume ratio was 1:1, the suspension was stirred at ...

Embodiment 3

[0065] This embodiment provides a sulfide solid state electrolyte Li 6 PS 5 The preparation method of I, concrete steps are as follows:

[0066] In a glove box, under argon atmosphere, weigh Li in a molar ratio of 3:1 2 S and P 2 S 5 , fully ground in an agate mortar and homogeneously dispersed in ultra-dry tetrahydrofuran by sonication. The ultrasonic time was 10 min and the frequency was 25 kHz.

[0067] (2) The mixture obtained in step (1) was stirred at room temperature overnight for 10 h under the protective conditions of anhydrous and oxygen-free to obtain Li with a mass fraction of 1% 3 PS 4 • 3THF / THF suspension.

[0068] (3) In a glove box filled with argon gas, weigh Li according to the molar ratio of 1:1 2 S and LiI were dissolved in anhydrous acetone to prepare a solution with a mass fraction of 3.74%.

[0069] (4) The solution obtained in (3) is added to the suspension obtained in (2). The volume ratio was 1:1, and the suspension was stirred overnight at...

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Abstract

The invention relates to a preparation method of sulfide solid electrolyte. The preparation method comprises the following steps: firstly, dissolving argyrodite type sulfide solid electrolyte raw materials in an ultra-dry solvent according to a certain proportion, and violently stirring so that the raw materials are fully and uniformly mixed and react; after the reaction is finished, unreacted residual solids are removed through centrifugation, a solution is collected, and a solvent is removed to obtain powder; and finally, sintering the dried powder in a vacuum sealed quartz tube to obtain the argyrodite type sulfide solid electrolyte. The preparation method disclosed by the invention solves the problems of high energy consumption caused by a traditional solid-state method, non-uniform mixing of raw materials for preparing the sulfide electrolyte and the like, and can improve the conductivity of the prepared sulfide electrolyte.

Description

technical field [0001] The invention belongs to the technical field of solid-state electrolytes, in particular to a preparation method of a sulfide solid-state electrolyte, and in particular to a preparation method of a liquid-phase method for mass-preparation of arginine-type sulfide solid-state electrolyte. Background technique [0002] At present, lithium-ion batteries have been commercialized, but traditional lithium-ion batteries have obvious safety hazards due to the use of liquid electrolytes. For example, liquid organic electrolytes are flammable, volatile, and easy to corrode. In contrast, the solid electrolyte used in all-solid-state batteries is non-flammable and non-volatile, which ensures the safety of the battery, and can also avoid the problem of short battery life caused by drying up of the liquid electrolyte during the battery cycle. [0003] Among the developed solid-state electrolytes, sulfide solid-state electrolytes have outstanding advantages in solid-s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562
CPCH01M10/0562
Inventor 张希朱金辉陈振营
Owner SHANGHAI FIRM-LITHIUM NEW ENERGY TECH CO LTD
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