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Nb and Ta co-doped garnet-type LLZO solid electrolyte and preparation method thereof

A solid electrolyte and garnet-type technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., can solve problems such as explosion, easy corrosion, and flammability of organic electrolytes

Inactive Publication Date: 2019-06-25
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, current commercial lithium-ion batteries have some serious drawbacks: the organic electrolyte used has potential safety hazards of flammability, corrosion, and even explosion
Although Ta 5+ Doped LLZO has high room temperature ionic conductivity, but tantalum sources are expensive

Method used

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  • Nb and Ta co-doped garnet-type LLZO solid electrolyte and preparation method thereof
  • Nb and Ta co-doped garnet-type LLZO solid electrolyte and preparation method thereof
  • Nb and Ta co-doped garnet-type LLZO solid electrolyte and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] According to the stoichiometric ratio of the final product and an excess of 10% of the lithium source, lithium carbonate Li 2 CO 3 , Lanthanum Oxide La 2 o 3 , Zirconia ZrO 2 , niobium oxide Nb 2 o 5 and tantalum oxide Ta 2 o 5 Mix the powder evenly to obtain a mixed powder. The particle sizes of the five powders are 5 μm, 10 μm, 0.5 μm, 10 μm, and 10 μm, and then weigh about 10 g of the mixed powder and place it in a ball mill made of zirconia. 300%) isopropanol and an appropriate amount of zirconia balls for ball milling, the ball mill speed is 200 rpm, and the ball milling time is 12 hours. After ball milling, the mixed materials were put into a drying oven and dried at 80°C for 6 hours. Then pre-fired at 900°C for 4h, then ball milled and dried, weighed 3.0g of the dried mixture and put it into a mortar, added 0.3g (10%) of a 10% PVA aqueous solution, ground for 15 minutes, and then the mixture The material is placed in a steel mold, and the green body is o...

Embodiment 2

[0034] According to the stoichiometric ratio of the final product and an excess of 15% of the lithium source, lithium carbonate Li 2 CO 3 , Lanthanum Oxide La 2 o 3 , Zirconia ZrO 2 , niobium oxide Nb 2 o 5 and tantalum oxide Ta 2 o 5 Mix the powder evenly to obtain a mixed powder. The particle sizes of the five powders are 10 μm, 10 μm, 1 μm, 10 μm, and 5 μm, and then weigh about 10 g of the mixed powder and place it in a ball mill made of zirconia. Add 20 g (200% ) isopropanol and an appropriate amount of zirconia balls for ball milling, the ball mill speed is 200 rpm, and the ball milling time is 16 hours. After ball milling, the mixed material was put into a drying oven and dried at 80°C for 12 hours. Then pre-fired at 1100°C for 1h, then ball milled and dried, weighed 3.0g of the dried mixture and put it into a mortar, added 0.3g (10%) of a 15% PVA aqueous solution, ground for 15 minutes, and then the mixture The material is placed in a steel mold, and the green ...

Embodiment 3

[0036] According to the stoichiometric ratio of the final product and an excess of 12% of the lithium source, lithium carbonate Li 2 CO 3 , Lanthanum Oxide La 2 o 3 , Zirconia ZrO 2 , niobium oxide Nb 2 o 5 and tantalum oxide Ta 2 o 5 Mix the powder evenly to obtain a mixed powder. The particle sizes of the five powders are 10 μm, 10 μm, 0.5 μm, 10 μm, and 10 μm. Then weigh about 10 g of the mixed powder and place it in a ball mill made of zirconia. Add 20 g (200 %) isopropanol and an appropriate amount of zirconia balls for ball milling, the ball mill speed is 300 rpm, and the ball milling time is 24 hours. After ball milling, the mixed material was put into a drying oven and dried at 80°C for 10 hours. Then pre-fired at 900°C for 4h, then ball milled and dried, weighed 3.0g of the dried mixture and put it into a mortar, added 0.3g (10%) of a 12% PVA aqueous solution, ground for 15 minutes, and then the mixture The material is placed in a steel mold, and the green bo...

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Abstract

The invention provides an Nb and Ta co-doped garnet-type LLZO solid electrolyte and a preparation method thereof. The solid electrolyte can be widely applied to an all-solid-state battery. The solid electrolyte has an expression of Li<7-x-y>La<3>Zr<2-x-y>Nb<x>Ta<y>O<12>, the values of x and y are 0 to 1.5, and 0.1<=x+y<=1.5. The Nb and Ta co-doped LLZO solid electrolyte with a cubic phase garnet structure can be prepared at a temperature of 800 to 1300 DEG C through a conventional solid phase method, a sol-gel method, a field assisted sintering method, a hot press sintering method and other methods, the room temperature lithium ion conductivity is 2.50*10<-4> S / cm to 1.40*10<-3> S / cm. Nb with a low price and Ta capable of improving the LLZO ion conductivity are adopted to together replacea Zr site, the LLZO with high ion conductivity and low cost can be obtained, and industrial production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of solid electrolyte preparation, and in particular relates to a novel Nb and Ta co-doped garnet type LLZO solid electrolyte and a preparation method thereof. Background technique [0002] Lithium-ion batteries are favored by people for their high energy density, low self-discharge, and long cycle life. However, current commercial lithium-ion batteries have some serious drawbacks: the organic electrolyte used has potential safety hazards of flammability, corrosion, and even explosion. In recent years, news of mobile phone batteries and electric vehicle batteries burning and exploding has been reported from time to time. [0003] The use of solid electrolytes instead of organic electrolytes and the assembly of positive and negative electrodes into all-solid lithium batteries can fundamentally solve the safety hazards of lithium-ion batteries, while further improving energy density and simplifying assembly. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/058H01M10/0525
CPCY02E60/10Y02P70/50
Inventor 陈斐向兴沈强张联盟
Owner WUHAN UNIV OF TECH
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