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Preparation method of sulfide solid electrolyte

A technology of solid electrolyte and solid electrolyte, applied in solid electrolyte, non-aqueous electrolyte, circuit, etc., can solve problems such as deformation and cracking, achieve high ion conductivity, improve crystallinity and density

Pending Publication Date: 2022-04-29
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention mainly aims at the deformation and cracking of the sulfur-argentite solid electrolyte during the sintering process, and at the same time can further improve the compactness of the sulfur-argentite solid electrolyte to increase the ion conductivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) The first step Li 6 P.S. 5 Preparation of Cl plain embryo, raw material Li 2 S, LiCl, P 2 S 5 Mix according to the molar fraction of 5:2:1, put it into a stainless steel ball mill tank with an air valve, and then put it into zirconia balls, the ball-to-material ratio is 20:1, fix it in a planetary ball mill and mill it at 550rpm / min for 24h to obtain Li 6 P.S. 5 Cl powder, weigh 150mg Li 6 P.S. 5 The Cl powder is pressed into an electrolyte sheet blank with a diameter of 10mm and a thickness of 1.2mm by using a cold press under a pressure greater than 360Mpa.

[0026] 2) The second step is a sintering process. The quartz tube containing the electrolyte sheet is heated to 500°C in a box furnace, the heating rate is 1°C / min, the holding time is 6h, and it is cooled to room temperature with the furnace.

[0027] 3) The third step is the second sintering process. The electrolyte sheet obtained by the first sintering is crushed and ground to powder, and the tube i...

Embodiment 2

[0029] 1) The first step Li 6 P.S. 5 Preparation of Cl plain embryo, raw material Li 2 S, LiCl, P 2 S 5 Mix according to the molar fraction of 5:2:1, put it into a stainless steel ball mill tank with an air valve, and then put it into zirconia balls, the ball-to-material ratio is 20:1, fix it in a planetary ball mill and mill it at 550rpm / min for 24h to obtain Li 6 P.S. 5 Cl powder, weigh 150mg Li 6 P.S. 5 The Cl powder is pressed into an electrolyte sheet blank with a diameter of 10mm and a thickness of 1.2mm by using a cold press under a pressure greater than 360Mpa.

[0030] 2) The second step is a sintering process. The quartz tube containing the electrolyte sheet is heated to 500°C in a box furnace, the heating rate is 1°C / min, the holding time is 6h, and it is cooled to room temperature with the furnace.

[0031] 3) The third step is the second sintering process. The electrolyte sheet obtained by the first sintering is crushed and ground to powder, and the tube i...

Embodiment 3

[0033] 1) The first step Li 6 P.S. 5 Preparation of Cl plain embryo, raw material Li 2 S, LiCl, P 2 S 5Mix according to the molar fraction of 5:2:1, put it into a stainless steel ball mill tank with an air valve, and then put it into zirconia balls, the ball-to-material ratio is 20:1, fix it in a planetary ball mill and mill it at 550rpm / min for 24h to obtain Li 6 P.S. 5 Cl powder, weigh 150mg Li 6 P.S. 5 The Cl powder is pressed into an electrolyte sheet blank with a diameter of 10mm and a thickness of 1.2mm by using a cold press under a pressure greater than 360Mpa.

[0034] 2) The second step is a sintering process. The quartz tube containing the electrolyte sheet is heated to 500°C in a box furnace with a heating rate of 1°C / min and a holding time of 10h, and then cooled to room temperature with the furnace.

[0035] 3) The third step is the second sintering process. The electrolyte sheet obtained by the first sintering is crushed and ground to powder, and the tube...

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Abstract

The invention relates to a preparation method of an inorganic sulfide solid electrolyte, and belongs to the field of lithium ion batteries. Aiming at the defects that a primary solid-phase sintering method of argyrodite solid electrolyte Li6PS5Cl is easy to deform, generate pores, curl and the like in the preparation process, improvement is carried out on the basis of a primary sintering preparation method, and a novel secondary sintering preparation method is obtained. The method is characterized in that a solid electrolyte sheet obtained by primary sintering is crushed and then tabletted again, and is sintered again at a slightly high temperature, and the novel process is beneficial to homogenization of the grain size, enlargement of the overall size of the grains and improvement of the crystallinity and density. Meanwhile, residual gas which is not volatilized in one-time sintering can be eliminated, deformation and defects of an electrolyte sheet are avoided, the obtained solid electrolyte is more uniform in surface and more compact in structure, subsequent characterization and electrochemical testing are facilitated, and the ionic conductivity of the sulfide solid electrolyte can also be improved.

Description

Technical field: [0001] The invention relates to the preparation of an all-solid-state battery in the field of lithium-ion batteries, and relates to the preparation of an inorganic sulfide solid electrolyte. Background technique: [0002] Today lithium-ion batteries have occupied the consumer market in new energy vehicles and electronics. Lithium-ion batteries using organic liquid electrolytes are prone to safety accidents such as electrolyte leakage and battery explosion due to the presence of lithium dendrites. These safety concerns can be alleviated by using inorganic solid-state electrolytes. Compared with conventional organic electrolytes, solid electrolytes can prevent the formation of lithium dendrites and withstand high voltages above 5 V. In addition, reduced packaging requirements also potentially improve gravimetric and volumetric energy densities. [0003] The advantages of sulfide solid electrolytes are easy molding and high lithium ion conductivity. Among t...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0562H01M10/0525H01M2300/0068Y02E60/10
Inventor 薛文东赵晨光
Owner UNIV OF SCI & TECH BEIJING
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