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Solid electrolyte, preparation method thereof and solid-state battery

A solid electrolyte and product technology, applied in the direction of non-aqueous electrolyte battery, electrolyte battery manufacturing, secondary battery, etc., can solve the problems of hindering the conductivity of electrolyte lithium ions, loss of electrolyte powder, low efficiency, etc., suitable for large-scale production , strong competitiveness, and the effect of inhibiting growth

Active Publication Date: 2020-11-17
CHINA AVIATION LITHIUM BATTERY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the process of mechanical crushing, it is easy to introduce a large amount of impurities and lose a certain amount of electrolyte powder, resulting in low efficiency.
At the same time, the grain boundaries between the particles formed by sintering at high temperature will not disappear in the mechanical crushing and ball milling process, and the existence of grain boundaries will seriously hinder the lithium ion conductivity of the electrolyte.

Method used

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  • Solid electrolyte, preparation method thereof and solid-state battery
  • Solid electrolyte, preparation method thereof and solid-state battery
  • Solid electrolyte, preparation method thereof and solid-state battery

Examples

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preparation example Construction

[0016] The preparation method of the solid electrolyte of the present invention comprises: a primary hydrogen crushing step, wherein the raw material of the polycrystalline solid electrolyte is subjected to hydrogen crushing treatment to obtain a product after the primary treatment.

[0017] "Hydrogen crushing" in this patent refers to the process of crushing particles by utilizing the brittleness of metal hydrides.

[0018] to combine figure 1 Explain the working principle of the preparation method of the present invention. Such as figure 1 As shown, when the polycrystalline solid electrolyte is sintered at high temperature in a hydrogen-containing atmosphere, hydrogen will permeate and accumulate at the grain boundaries, phase boundaries and defects of the electrolyte, which will cause the electrolyte to be hydrogenated to form a brittle metal hydride, and the formed hydride Volume expansion and internal stress are generated in the local area. When the internal stress exce...

Embodiment 1

[0024] Embodiment 1: Garnet type Li 7 La 3 Zr 2 o 12 Preparation of solid electrolyte

[0025] Step 1, according to the mass molar ratio Li:La:Zr=7:3:2, weigh LiOH·H 2 O, La 2 o 3 (pretreatment at 900°C for 12h), ZrO 2 , where the lithium source is in excess of 10%, to supplement the loss during the high temperature sintering process.

[0026] Step 2: Mix the weighed reagent and solvent isopropanol into a ball mill jar, and run the high-energy ball mill for 6 hours under the condition of using zirconia balls as grinding beads, and set the average speed at 400r / min. Then place the slurry in a blast drying oven at 100°C to dry the slurry, then place it in a crucible for calcination at 1000°C for 12 hours, and cool to obtain product A.

[0027] Step 3, put the product A in a pressure vessel and pass through a hydrogen-containing gas to raise the temperature to 700° C., keep the temperature for 3 hours, and obtain the product B with a hydrogen partial pressure of 5 atmosph...

Embodiment 2

[0030] Embodiment 2: Garnet type Li 6.75 La 3 Zr 1.75 Nb 0.25 o 12 Preparation of solid electrolyte

[0031] Step 1, according to the mass molar ratio Li:La:Zr:Nb=6.75:3:1.75:0.25, weigh LiOH·H 2 O, La 2 o 3 (pretreatment at 900°C for 12h), ZrO 2 and Nb 2 o 5 , where the lithium source is in excess of 10%, to supplement the loss in the high-temperature sintering process.

[0032] Step 2 is the same as that of Example 1.

[0033] Step 3 is different from Example 1 in that the temperature is 600° C., the temperature is kept for 1 hour, and the hydrogen partial pressure is 1 atmosphere.

[0034] Step 4 is the same as that of Example 1.

[0035] Step 5 is the same as that in Example 1.

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Abstract

The invention discloses a solid electrolyte, a preparation method thereof and a battery containing the solid electrolyte. The preparation method of the solid electrolyte comprises the following steps:carrying out hydrogen decrepitation treatment on a polycrystalline solid electrolyte raw material to obtain a product after primary treatment; the solid electrolyte is prepared by hydrogen decrepitation, namely, hydrogen is introduced in the high-temperature sintering process of electrolyte particles, metal hydride is formed at the grain boundary, and the electrolyte is prepared by utilizing thehydrogen embrittlement phenomenon of the metal hydride. According to the method, the grain boundary between electrolyte particles can be eliminated, and the lithium ion conduction performance of the electrolyte is greatly improved; and when the electrolyte is applied to a solid-state battery, the growth of lithium dendrites can also be inhibited by eliminating grain boundaries among electrolyte particles. According to the method, a mechanical crushing process is not needed, introduction of impurities is avoided, the preparation process is simplified, the method is suitable for large-scale production, and strong competitiveness is provided for the future solid-state battery market.

Description

technical field [0001] The invention belongs to the field of solid-state electrolyte batteries, and in particular relates to a solid-state electrolyte, a preparation method thereof and a solid-state battery. Background technique [0002] The particles of inorganic solid electrolyte materials will agglomerate and agglomerate during the high-temperature sintering process. It is necessary to mechanically crush the electrolyte block to obtain coarse particles, and then refine the electrolyte powder by ball milling or dry spraying. However, in the process of mechanical crushing, it is easy to introduce a large amount of impurities and lose a certain amount of electrolyte powder, resulting in low efficiency. At the same time, the grain boundaries between the particles formed by sintering at high temperature will not disappear in the mechanical crushing and ball milling process, but the existence of grain boundaries will seriously hinder the lithium ion conductivity of the electrol...

Claims

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Application Information

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IPC IPC(8): C01G25/00C01G33/00C01G35/00H01M10/052H01M10/0562H01M10/058H01M10/42
CPCC01G25/006C01G33/006C01G35/006H01M10/0562H01M10/058H01M10/052H01M10/4235Y02E60/10Y02P70/50
Inventor 李旭王康平李洋曹晨
Owner CHINA AVIATION LITHIUM BATTERY RES INST CO LTD
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