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A method for preparing high-conductivity garnet-type electrolyte sheet at low temperature

A garnet-type, high-conductivity technology, applied in the direction of electrolytes, circuits, electrical components, etc., can solve the problems of difficult control of solid electrolyte components, volatilization of lithium components, etc., to facilitate large-scale production, low synthesis temperature, and high conductivity rate effect

Active Publication Date: 2021-09-28
北京金科创能新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the high-temperature solid-state reaction method is often used to prepare Li 7 La 3 Zr 2 o 12 and doped Li 7 La 3 Zr 2 o 12 Garnet-type solid electrolyte, but the firing temperature is too high, which causes the lithium component in the composition to volatilize, forming a low-conductivity impurity phase, and the prepared solid electrolyte composition is difficult to control

Method used

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  • A method for preparing high-conductivity garnet-type electrolyte sheet at low temperature
  • A method for preparing high-conductivity garnet-type electrolyte sheet at low temperature
  • A method for preparing high-conductivity garnet-type electrolyte sheet at low temperature

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Weigh lithium hydroxide, lanthanum hydroxide, zirconium oxide, germanium oxide, and tantalum pentoxide according to the stoichiometric ratio, and add lithium hydroxide to the ball mill tank with an excess of 10wt.%, and add an appropriate amount of isopropanol to ball mill for 10 hours , Dry at 75°C for 12h.

[0022] 2. Calcining the obtained powder at 900° C. for 10 h to prepare solid electrolyte powder.

[0023] 3. Ball mill the burnt powder again, dry it at 75°C, and press it into tablets under isostatic pressure at 300MPa. The solid electrolyte sheet is placed on a high-purity corundum ceramic plate covered with solid electrolyte powder, and the electrolyte sheet is buried with the electrolyte powder. Cover with an arc-shaped crucible, heat up to 1150°C at 5°C / min for sintering, and hold for 10 hours to prepare the required Li 6.6 La 3 Zr 1.4 Ta 0.4 Ge 0.2 o 12 Solid Electrolyte Sheet.

[0024] 4. Use 400-mesh SiC sand to polish the solid electrolyte shee...

Embodiment 2

[0026] 1. Weigh lithium carbonate, lanthanum oxide, zirconium oxide, tungsten oxide, and tantalum pentoxide according to the stoichiometric ratio, wherein the excess lithium is 15wt.%, and add an appropriate amount of alumina at the same time, and add the above raw materials into the ball mill tank, Add an appropriate amount of n-butanol to ball mill for 12 hours, and dry at 80°C for 12 hours.

[0027] 2. Calcining the obtained powder at 900° C. for 12 hours to prepare solid electrolyte powder.

[0028] 3. Ball mill the burnt powder again, dry it at 80°C, press isostatically at 200MPa to form a tablet. The solid electrolyte sheet is placed on a high-purity corundum ceramic plate covered with solid electrolyte powder, and the electrolyte sheet is buried with the electrolyte powder. Cover with an arc-shaped crucible, heat up to 1200°C at 3°C / min for sintering, and hold for 10 hours to prepare the required Li 6.4 La 3 Zr 1.4 Ta 0.5 W 0.1 o 12 Solid Electrolyte Sheet.

[0...

Embodiment 3

[0031] 1. Weigh lithium carbonate, lanthanum nitrate, zirconium oxide nitrate, germanium oxide, tantalum pentoxide, and tungsten oxide according to the stoichiometric ratio, among which lithium hydroxide is in excess of 10wt.%. , Dry at 55°C for 12h.

[0032] 2. Calcinate the obtained powder at 850°C for 10 hours.

[0033] 3. Ball-mill the burnt powder again, dry it at 55°C, press isostatically at 200MPa to form a tablet. The solid electrolyte sheet is placed on a high-purity corundum ceramic plate covered with solid electrolyte powder, and the electrolyte sheet is buried with the electrolyte powder. Cover with an arc-shaped crucible, heat up to 1050°C at 5°C / min for sintering, and hold for 10 hours to prepare the required Li 6.6 La 3 Zr 1.4 Ta 0.3 W 0.1 Ge 0.2 o 12 Solid Electrolyte Sheet.

[0034] 4. Use 1500-mesh SiC sand solid electrolyte sheet to polish and silver-plate it, and test its electrochemical impedance.

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Abstract

The invention provides a method for preparing a high-conductivity garnet-type electrolyte sheet at low temperature, which comprises the following steps: adding the raw materials required for the synthesis of solid electrolyte powder into a ball milling tank, adding an appropriate amount of grinding aid, and ball-milling the obtained powder after drying After the body is roasted at 800-950°C, grinding aids are added to ball mill again, and the dried powder after ball milling is pressed into tablets by isostatic pressing. Place the solid electrolyte sheet on a high-purity corundum ceramic plate covered with solid electrolyte powder, bury the solid electrolyte sheet with the electrolyte powder, cover the solid electrolyte sheet to be fired with a crucible upside down, and roast at low temperature to prepare the required pomegranate Stone-shaped solid electrolyte sheet. The invention has low synthesis temperature, is convenient for controlling the amount of lithium in the solid electrolyte component, has a simple synthesis process, and can prepare a high-density and high-conductivity garnet-type solid electrolyte sheet at low temperature.

Description

technical field [0001] The invention belongs to the field of batteries, in particular to a solid electrolyte with stable interface and high conductivity. Background technique [0002] Has high conductivity (~10 -4 S / cm) Li 7 La 3 Zr 2 o 12 The garnet-type solid electrolyte has a relatively stable interface with metal Li and has good chemical stability in the air. It has a good application prospect in the research and development of high energy density and safe all-solid-state batteries. Li 7 La 3 Zr 2 o 12 There are tetragonal phases and cubic phases. Studies have shown that cubic phases with high electrical conductivity are easily synthesized at high temperatures, but a certain amount of tetragonal phases appears during cooling. To stabilize Li 7 La 3 Zr 2 o 12 Phase, using Al 3+ , B 3+ , Ga 3+ 、 Ta 5+ and other elements for doping, through the comparison of research results, Ta 5+ The doping of ions helps to improve the conductivity of the solid electroly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562
CPCH01M10/0562H01M2300/0071Y02E60/10
Inventor 李栋雷超其他发明人请求不公开姓名
Owner 北京金科创能新材料科技有限公司
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