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Method for liquid-phase preparation of doped argyrodite type sulfide solid electrolyte with high ionic conductivity

A technology of solid electrolyte and silver germanium ore, which is applied in the direction of electrochemical generators, circuits, electrical components, etc., can solve the problems of time-consuming, unscaled production, and tediousness, and achieve small particles, improve ionic conductivity and The effect of air stability and easy tablet molding

Pending Publication Date: 2022-07-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is that at present, the doping and modification of silver-silver-germanium ore-type sulfide solid electrolyte can only be done through mechanical ball milling, which is cumbersome and time-consuming, and does not have the prospect of large-scale production.

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  • Method for liquid-phase preparation of doped argyrodite type sulfide solid electrolyte with high ionic conductivity
  • Method for liquid-phase preparation of doped argyrodite type sulfide solid electrolyte with high ionic conductivity
  • Method for liquid-phase preparation of doped argyrodite type sulfide solid electrolyte with high ionic conductivity

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Embodiment 1

[0041] The present embodiment utilizes liquid phase to prepare a doped high ionic conductivity argentine-type sulfide solid state electrolyte, and the preparation method includes the following steps:

[0042] 1) In the glove box, weigh 2.3g of lithium sulfide and 2.2g of phosphorus pentasulfide, add the two medicines to 45g of anhydrous acetonitrile, sonicate for 20 minutes with a power of 50W and a frequency of 50Hz, and then place the ultrasonic solution at 50°C. The reaction was stirred for 12 hours, and the color of the solution changed from light yellow to light blue.

[0043] 2) In the glove box, weigh 2.7g of lithium iodide, 1.7g of antimony sulfide, and 0.3g of sublimated sulfur into the light blue solution after the reaction in step 1), and continue to stir the reaction at 50 ° C for 12 hours to obtain the reaction after the reaction. The solution.

[0044] 3) Transfer the reacted solution to an open container, dry and remove the acetonitrile at a temperature of 80°C...

Embodiment 2

[0049] The present embodiment utilizes liquid phase to prepare a doped high ionic conductivity argentine-type sulfide solid state electrolyte, and the preparation method includes the following steps:

[0050] 1) In the glove box, weigh 2.3g of lithium sulfide and 2.2g of phosphorus pentasulfide, add the two medicines to 45g of anhydrous acetonitrile, sonicate for 20 minutes with a power of 50W and a frequency of 50Hz, and then place the ultrasonic solution at 50°C. The reaction was stirred for 12 hours, and the color of the solution changed from light yellow to light blue.

[0051] 2) In the glove box, weigh 2.7 g of lithium iodide, 1.3 g of arsenic sulfide, and 0.3 g of sublimated sulfur into the light blue solution after the reaction in step 1), and continue to stir the reaction at 50 ° C for 12 hours to obtain the reaction. the solution after.

[0052] 3) Transfer the reacted solution to a petri dish, dry it at 80°C to remove acetonitrile, and then sinter the obtained powd...

Embodiment 3

[0054] The present embodiment utilizes liquid phase to prepare a doped high ionic conductivity argentine-type sulfide solid state electrolyte, and the preparation method includes the following steps:

[0055] 1) In the glove box, weigh 2.3g of lithium sulfide and 2.2g of phosphorus pentasulfide, add the two medicines to 45g of anhydrous acetonitrile, sonicate for 20 minutes with a power of 50W and a frequency of 50Hz, and then place the ultrasonic solution at 50°C. The reaction was stirred for 12 hours, and the color of the solution changed from light yellow to light blue.

[0056] 2) In the glove box, weigh 2.7 g of lithium iodide, 1.0 g of antimony sulfide, and 0.2 g of sublimated sulfur into the light blue solution after the reaction in step 1). The solution.

[0057] 3) Transfer the reacted solution to a petri dish, dry at 80°C to remove acetonitrile, and then sinter the obtained powder at 450°C for 2 hours at a heating / cooling rate of 2°C / min to obtain crystalline Sb-dop...

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Abstract

The invention belongs to the technical field of solid electrolyte, and discloses a method for preparing doped argyrodite type sulfide solid electrolyte with high ionic conductivity in a liquid phase. The method comprises the following steps: 1) dispersing lithium sulfide and phosphorus pentasulfide in an organic solvent, heating, stirring and reacting to obtain a precursor solution containing Li3PS4; 2) mixing lithium iodide, powdered sulfur and an additive with the precursor solution, heating and stirring for reaction, and removing the organic solvent to obtain powder; and 3) sintering the powder in a protective atmosphere to obtain the argyrodite type sulfide solid electrolyte, and the additive is one or more of SiS2, GeS2, SnS2, As2S3 and Sb2S3. The method is simple, the prepared argyrodite type sulfide electrolyte is subjected to element doping in the thermal crystallization process, and the ionic conductivity and air stability of the electrolyte are improved. The method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of solid electrolyte materials for solid-state batteries, and in particular relates to a method for preparing a doped high-ionic-conductivity sapphire-type sulfide solid-state electrolyte in a liquid phase. Background technique [0002] Due to the advantages of high energy density and long cycle life, lithium-ion batteries are widely used in most portable electronic devices. However, traditional Li-ion batteries have huge safety hazards due to the use of volatile and flammable liquid electrolytes, which limit the further development of Li-ion batteries. All-solid-state batteries can well solve the safety problem of batteries due to the use of solid-state electrolytes with excellent thermal stability and good mechanical properties. Among many solid-state electrolytes, sulfide solid-state electrolytes have ionic conductivity comparable to that of liquid electrolytes, so they are considered to be solid-state e...

Claims

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Application Information

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IPC IPC(8): H01M10/0567H01M10/0568
CPCH01M10/0568H01M10/0567Y02E60/10
Inventor 王素清姬兵黄广苏苗苗
Owner SOUTH CHINA UNIV OF TECH
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