Preparation method of high-density garnet all-solid electrolyte under low temperature and application of high-density garnet all-solid electrolyte

A garnet-type, dense technology, applied in the direction of electrolytes, circuits, electrical components, etc., can solve the problem of low density and achieve the effect of promoting industrial application

Inactive Publication Date: 2019-08-16
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problem of low density under low-temperature sintering, the present invention provide...

Method used

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  • Preparation method of high-density garnet all-solid electrolyte under low temperature and application of high-density garnet all-solid electrolyte
  • Preparation method of high-density garnet all-solid electrolyte under low temperature and application of high-density garnet all-solid electrolyte
  • Preparation method of high-density garnet all-solid electrolyte under low temperature and application of high-density garnet all-solid electrolyte

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Embodiment 1

[0026] This embodiment prepares Li according to the following steps 7 La 3 Zr 2 o 12 Electrolyte sheet:

[0027] 1. Add LiOH·H 2 O, La 2 o 3 , ZrO 2 Weigh it according to the stoichiometric ratio, add it to the ball mill tank, and add an excess of 10% Li, add an appropriate amount of isopropanol to ball mill for 24 hours, and dry it at 70 °C for 1 hour after the end.

[0028] 2. Take out the obtained powder, put it into a corundum porcelain boat for compaction, then raise the temperature to 900°C at a rate of 2°C / min, and finish the heat preservation for 9 hours.

[0029] 3. Take part of the obtained precursor powder and process it again with high-energy ball milling for 45 minutes. After that, mix the precursor powder after high-energy ball milling treatment with that without high-energy ball milling in a mass ratio of 3:7, and use a powder tablet press Compressed into tablets at 30MPa.

[0030] 4. Put the electrolyte sheet into the corundum porcelain boat, and sprea...

Embodiment 2

[0032] This embodiment prepares Li according to the following steps 6.7 La 3 Zr 1.7 Nb 0.3 o 12 Electrolyte sheet:

[0033] 1. Will Li 2 CO 3 , La 2 o 3 , ZrO 2 , Nb 2 o 5 Weigh it according to the stoichiometric ratio, add it to the ball mill jar, and add an excess of 15% Li, add an appropriate amount of isopropanol and ball mill it for 24 hours, and then dry it at 80°C for 1 hour.

[0034] 2. Take out the obtained powder, put it into a corundum porcelain boat for compaction, then raise the temperature to 900°C at a rate of 2°C / min, and finish the heat preservation for 9 hours.

[0035] 3. Take part of the obtained precursor powder and process it again with high-energy ball milling for 45 minutes, then mix the precursor powder after high-energy ball milling treatment with that without high-energy ball milling in a mass ratio of 4:6, and use a powder tablet press Compressed into tablets at 30MPa.

[0036] 4. Put the electrolyte sheet into the corundum porcelain bo...

Embodiment 3

[0038] This embodiment prepares Li according to the following steps 6.5 al 0.1 La 3 Zr1.5 Ta 0.5 o 12 Electrolyte sheet:

[0039] 1. Will Li 2 CO 3 , La 2 o 3 , ZrO 2 、 Ta 2 o 5 Weigh it according to the stoichiometric ratio, add it to the ball mill tank, and add an excess of 10% Li, add an appropriate amount of isopropanol to ball mill for 24 hours, and dry it at 70 °C for 1 hour after the end.

[0040] 2. Take out the obtained powder, put it into a corundum porcelain boat for compaction, then raise the temperature to 850°C at a rate of 2°C / min, and finish the heat preservation for 12 hours.

[0041] 3. Take part of the obtained precursor powder and process it again with high-energy ball milling for 45 minutes. After that, mix the precursor powder after high-energy ball milling treatment with that without high-energy ball milling in a mass ratio of 3:7, and use a powder tablet press Compressed into tablets at 30MPa.

[0042] 4. Put the electrolyte sheet into the ...

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Abstract

The invention discloses a preparation method of a high-density garnet all-solid electrolyte under low temperature and an application of the high-density garnet all-solid electrolyte. The method comprises the following steps: 1) adding raw materials to a ball milling tank according to the stoichiometric ratio of LLZO, adding isopropanol as a grinding aid and carrying out ball milling and drying; 2)compacting the dried powders in a corundum porcelain boat, and then, carrying out heating and roasting to prepare LLZO precursor powders; 3) further milling a part of the LLZO precursor powders through high-energy ball milling; 4) mixing and pressing the LLZO precursor powders and the LLZO precursor powders obtained after high-energy ball milling into a sheet to obtain an electrolyte sheet; and 5) placing the electrolyte sheet into the corundum porcelain boat for powder embedded sintering to obtain a high-purity LLZO electrolyte sheet. Compared with other solid state sintering methods, the method is lower in sintering temperature and sheet compressing pressure of the garnet electrolyte sheet, thereby reducing production cost of the garnet electrolyte.

Description

technical field [0001] The invention relates to a method for preparing a solid electrolyte and its application, in particular to a method for sintering a high-density garnet solid electrolyte at low temperature and its application. Background technique [0002] Compared with other types of secondary batteries, lithium-ion batteries have the advantages of high discharge voltage, long cycle life, and high specific energy. At present, lithium-ion commercialized lithium-ion batteries use flammable and explosive organic electrolytes, so there are major safety issues. All-solid-state lithium-ion batteries use solid-state electrolytes to replace organic electrolytes, which fundamentally solves the safety problem. At the same time, the solid electrolyte has a better effect of inhibiting the growth of lithium dendrites, and metal lithium can be used as the negative electrode, which has a higher energy density. At present, the solid electrolytes that have been studied more are NASIC...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0071Y02E60/10
Inventor 张乃庆宋宁范立双
Owner HARBIN INST OF TECH
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