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Method for synthesizing sulfide solid electrolyte

A technology of solid electrolytes and sulfides, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve the problems of low ionic conductivity of sulfide solid electrolytes, limitations of sulfide solid electrolytes, etc.

Inactive Publication Date: 2021-05-07
SHANDONG RUIFU LITHIUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the ionic conductivity of the obtained sulfide solid electrolyte is low
[0006] All of the above methods require the use of high-purity lithium sulfide raw materials. The current high price of high-purity lithium sulfide severely limits the practical application of sulfide solid electrolytes. Therefore, the low-cost method for developing synthetic sulfide solid electrolytes is to promote sulfide electrolytes and sulfide solid state The key to the practical use of batteries

Method used

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  • Method for synthesizing sulfide solid electrolyte
  • Method for synthesizing sulfide solid electrolyte
  • Method for synthesizing sulfide solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under a dry argon atmosphere, according to Li 7 P 3 S 11 Composition ratio, weigh 0.8983g of lithium powder, 2.1373g of sulfur powder and 6.1644g of phosphorus pentasulfide to form a mixture with a total mass of 9.2g, of which the excess of sulfur powder is 3%, and place it in a ball mill tank for plasma ball milling for 4h. Under the protection of a dry nitrogen atmosphere, the ball-milled powder was heat-treated at 550°C for 1 hour, and then rapidly cooled to room temperature after heat treatment. The calcined powder was crushed by shearing to obtain Li 7 P 3 S 11 electrolyte. The Li measured by the electrochemical workstation 7 P 3 S 11 The electrolyte has an ionic conductivity of 1.9 mS / cm at 25 °C.

Embodiment 2

[0038] Under a dry argon atmosphere, according to Li 6 P.S. 5 Cl composition ratio, weigh 1.2358g of lithium powder, 2.9973g of sulfur powder, 3.9574g of phosphorus pentasulfide and 1.5095g of anhydrous lithium chloride to form a mixture with a total mass of 9.7g, place it in a ball mill tank for plasma ball milling for 3h, wherein the excess of sulfur powder is 5 %. Under the protection of a dry nitrogen atmosphere, the ball-milled powder was heat-treated at 450°C for 2 hours, and then rapidly cooled to room temperature after heat treatment. The calcined powder was crushed by shearing to obtain Li 6 P.S. 5 Cl electrolyte. The Li measured by the electrochemical workstation 6 P.S. 5 The ionic conductivity of the Cl electrolyte is 3.2 mS / cm at 25 °C.

Embodiment 3

[0040] Under a dry argon atmosphere, according to Li 9.54 Si 1.74 P 1.44 S 11.7 Cl0.3 Composition ratio, weigh 1.1833g lithium powder, 2.8694g sulfur powder, 2.9601g silicon disulfide, 2.9525g phosphorus pentasulfide and 0.2347g anhydrous lithium chloride to form a mixture with a total mass of 10.2g, place it in a ball mill tank for plasma ball milling for 3h, Among them, the excess of sulfur powder is 3%. Under the protection of a dry argon atmosphere, the ball-milled powder was heat-treated at 550°C for 1 hour, and then rapidly cooled to room temperature after heat treatment. The calcined powder is crushed by grinding to obtain Li 9.54 Si 1.74 P 1.44 S 11.7 Cl 0.3 electrolyte. The Li measured by the electrochemical workstation 9.54 Si 1.74 P 1.44 S 11.7 Cl 0.3 The ionic conductivity of the electrolyte is 3.0 mS / cm at 25 °C.

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Abstract

The invention relates to a method for synthesizing a sulfide solid electrolyte. The method comprises the following steps of: weighing raw materials according to a composition proportion of a sulfide solid electrolytic tank in a dry argon atmosphere, and performing plasma ball milling in a ball milling tank, wherein the raw materials comprise pure lithium, powdered sulfur and phosphorus pentasulfide; under the protection of a dry inert atmosphere, performing heat treatment on the powder obtained after ball milling in the step 1 at the temperature of 350-550 DEG C for 1-5 hours, and performing rapid shock cooling after heat treatment; and crushing and granulating the product subjected to heat treatment in the step 2 to obtain the sulfide electrolyte. The method does not need to adopt a lithium sulfide raw material, directly uses the pure lithium and sulfur powder which are low in price as raw materials, and adopts a plasma ball milling technology, so that the pure lithium, the sulfur powder and phosphorus pentasulfide raw materials can directly form a solid electrolyte precursor; and the performance of the synthesized solid electrolyte is equivalent to that of a solid electrolyte obtained by adopting an existing method.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a method for synthesizing a sulfide solid electrolyte. Background technique [0002] Lithium-ion batteries have been widely used in digital products, electric vehicles, energy storage power stations and other fields. Due to the use of liquid electrolyte in traditional lithium-ion batteries, the safety problem cannot be completely solved. Solid-state batteries, including all-solid-state batteries, can effectively solve the problem of battery safety due to the use of non-flammable solid-state electrolytes. Among the developed solid electrolytes, the sulfide solid electrolytes (Li-P-S, Li-P-S-Cl, Li-Ge-P-S Li-Sn-P-S, Li-Si-P-S-Cl) are known for their high room temperature conductivity, thermal With good stability and wide electrochemical window, it has outstanding advantages in high-power and room-temperature solid-state batteries, and is a solid-state electrolyte mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0562H01M10/0525H01M2300/0068Y02E60/10
Inventor 亓亮彭文修吕延鹏代文彬宋大卫
Owner SHANDONG RUIFU LITHIUM IND
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