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A kind of preparation method of sulfur silver germanium ore type sulfide solid state electrolyte

A solid-state electrolyte, silver-sulfur germanium ore technology, applied in the field of lithium-ion batteries, can solve the problems of low ionic conductivity of solid-state electrolyte, easy to stick to the tank wall and spherical surface, unable to obtain the expected crystal phase, so as to reduce CO2 escape. , to avoid uneven mixing of materials, to avoid the effect of solvent difficult to remove

Active Publication Date: 2022-06-24
湖南恩捷前沿新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the solid-phase method is mainly heat treatment after high-energy ball milling. The raw materials are easily bonded to the tank wall and the surface of the ball during the ball milling process, and the distribution of raw materials is uneven, and the expected crystal phase cannot be obtained.
Liquid phase method due to P 2 S 5 The raw materials are difficult to dissolve, the reaction time is long, and the ionic conductivity of the obtained solid electrolyte is generally low

Method used

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  • A kind of preparation method of sulfur silver germanium ore type sulfide solid state electrolyte

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Effect test

Embodiment 1

[0027] Weigh 2N pure reagent Li according to the stoichiometric ratio of 5:2:6:2 2 O 2 , P, CS 2 and LiCl, put into a zirconia ball mill with an air valve in turn, add zirconia balls with a ball-to-material ratio of 40:1, seal the ball mill and vacuumize it, vacuum degree 6 PS 5 Cl solid electrolyte powder. figure 1 is the XRD pattern of the solid electrolyte powder. The solid electrolyte powder is pressed under a pressure of 200Mpa, and the pressure is maintained for 3 minutes to obtain a solid electrolyte sheet. The whole process was carried out under an argon protective atmosphere. The lithium electrical conductivity of the solid electrolyte sheet at room temperature is 3.2×10 -3 S cm -1 .

Embodiment 2

[0029] Weigh 2N pure reagent Li according to the stoichiometric ratio of 5:2:5:2 2 O 2 , P, CS 2 and LiCl, put into a zirconia ball mill with an air valve in turn, add zirconia balls with a ball-to-material ratio of 30:1, seal the ball mill and vacuumize it, the degree of vacuum is less than -0.09MPa, and then put it into a planetary ball mill Carry out ball milling, the ball milling speed is 800r / min, the ball milling is 15 hours, and the ball mill tank is evacuated every 3 hours, and the vacuum degree is less than -0.09MPa. Then take out the initial electrolyte material and put it in an electric furnace to heat up to 300°C at a rate of 10°C / min, keep the temperature for 3 hours, put it into a mortar for natural cooling and grind it, and pass through a 400-mesh sieve to obtain Li 6 PS 5 Cl solid electrolyte powder. The solid electrolyte powder is pressed under a pressure of 200Mpa, and the pressure is maintained for 3 minutes to obtain a solid electrolyte sheet. The whol...

Embodiment 3

[0031] Weigh 2N pure reagent Li according to the stoichiometric ratio of 5:1:6:2 2 O.P 2 O 5 , CS 2 and LiCl, put into a zirconia ball mill with an air valve in turn, add zirconia balls with a ball-to-material ratio of 40:1, seal the ball mill and vacuumize it, vacuum 6 PS 5 Cl solid electrolyte powder. figure 1 is the XRD pattern of the solid electrolyte powder. The solid electrolyte powder is pressed under a pressure of 200Mpa and maintained for 3 minutes to obtain a solid electrolyte sheet. The whole process was carried out under an argon protective atmosphere. The lithium conductivity of the solid electrolyte sheet at room temperature is 1.3×10 -3 S cm -1 .

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Abstract

The invention discloses a CS 2 The invention discloses a preparation method of a sulfide solid state electrolyte which combines wet ball milling and solid phase ball milling as raw materials and solvents. The present invention uses the cheap Li 2 o 2 or Li 2 O, P or P 2 o 5 、CS 2 And LiX (X is Cl, Br or I) as raw materials, avoiding the expensive Li 2 The use of S, the preparation of solid electrolytes by the combination of vacuum wet ball milling and solid phase ball milling, CS 2 Even the raw material is also a solvent, the raw material has strong reactivity and high utilization rate, and the preparation method is simple without high-temperature sintering. The prepared sulfur-argentite-type solid electrolyte has high ion conductivity and a wide electrochemical window. It is applied to the preparation of all-solid-state batteries, which has high safety, high energy density, and excellent cycle stability.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method of a silver-germanite-type sulfide solid-state electrolyte. Background technique [0002] With the increasing demand for energy storage systems with high energy density and high safety, the development of secondary all-solid-state battery technology has received extensive attention. As a key component of all-solid-state batteries, solid-state electrolytes with high ionic conductivity can effectively eliminate the inherent safety problems of flammable organic electrolytes in traditional lithium-ion batteries, and also make battery packaging easier and more efficient, thereby further improving the energy density of the battery system. . [0003] So far, many superionic conductors have been regarded as candidate materials for solid-state electrolytes of all-solid-state lithium batteries, among which sulfide solid-state electrolytes and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B30/00C01D15/00H01M10/0525H01M10/0562
CPCC04B30/00C01D15/00H01M10/0562H01M10/0525H01M2300/0068C01P2006/40C04B2111/00844C04B22/16Y02E60/10
Inventor 刘芳洋吕娜胡雅琪蒋良兴贾明张宗良
Owner 湖南恩捷前沿新材料科技有限公司
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