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Industrialized preparation method of tantalum-aluminum-codoped lithium-lanthanum zirconate solid-state electrolyte

A solid-state electrolyte, lithium lanthanum zirconate technology, used in chemical instruments and methods, tantalum compounds, inorganic chemistry, etc., can solve the problems of high experimental repeatability, high ionic conductivity, high product density, and easy generation of miscellaneous phase conductivity. , to achieve the effect of simple preparation process, improved electrical conductivity and high density

Inactive Publication Date: 2018-12-21
淮安新能源材料技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the problems of easy generation of impurity phases and low electrical conductivity during the synthesis and preparation of lanthanum lithium zirconate solid electrolyte, and provides an industrialized preparation method for co-doping of tantalum and aluminum elements, solid-phase sintering at normal pressure, and simple preparation process. The cost of the equipment is low and easy to operate. Although the sintering time is long, the final product has high density, good experimental repeatability and high ion conductivity.

Method used

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  • Industrialized preparation method of tantalum-aluminum-codoped lithium-lanthanum zirconate solid-state electrolyte
  • Industrialized preparation method of tantalum-aluminum-codoped lithium-lanthanum zirconate solid-state electrolyte
  • Industrialized preparation method of tantalum-aluminum-codoped lithium-lanthanum zirconate solid-state electrolyte

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Experimental program
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Effect test

Embodiment 1

[0025] 14.49g (10% excess of Li source) lithium hydroxide monohydrate powder, 24.45g lanthanum oxide powder (the mass after sintering at 900 ℃ for 12h), 10.78g zirconium dioxide, 2.7625g (X=0.25) five Tantalum oxide and 50 ml of isopropanol were added, and then stirred evenly to ensure adequate mixing, and zirconia balls with a ball-to-material ratio of 5:1 were added and placed in a ball mill for 12 hours at 500 rpm. After the ball mill is finished, take it out and filter it, put it in an oven for 6 hours at 80°C, take it out and grind it with a mortar for 30 minutes after it is completely dried, and then sieve it after grinding it into powder. After collecting and sieving, the powder was placed in a magnesia crucible for calcination at 850°C for 12 hours. After cooling, it was taken out and ground again for 30 minutes to form a powder. Part of the powder was sieved and collected as master powder. Repeat the ball milling work for another part of the powder, weigh 0.51g of alu...

Embodiment 2

[0027]13.90g (10% excess of Li source) lithium hydroxide monohydrate powder, 24.45g lanthanum oxide powder (the mass after sintering at 900°C for 12h), 32.20g zirconium nitrate, 5.525g (X=0.5) pentoxide Add tantalum and 50ml of absolute ethanol, stir evenly to ensure full mixing, add zirconium dioxide balls with a ball-to-material ratio of 5:1 and place them in a ball mill for 12h at 500rpm. After the ball mill is finished, take it out and filter it, put it in an oven for 6 hours at 80°C, take it out and grind it with a mortar for 30 minutes after it is completely dried, and then sieve it after grinding it into powder. After collecting and sieving, the powder was placed in a magnesia crucible for calcination at 900°C for 9 hours. After cooling, it was taken out and ground again for 30 minutes to form a powder. Part of the powder was sieved and collected as master powder. Repeat the ball milling work for another part of the powder, weigh 0.51g of alumina into the obtained powde...

Embodiment 3

[0029] 19.15g (20% excess of Li source) lithium oxalate powder, 28.49g lanthanum hydroxide powder (the mass after sintering at 900℃ for 12h), 14.33g zirconium hydroxide, 2.21g (X=0.2) dioxide pentoxide Tantalum and 50 ml of isopropanol were added, and then stirred evenly to ensure adequate mixing, and zirconia balls with a ball-to-material ratio of 5:1 were added and placed in a ball mill for 12 hours at 500 rpm. After the ball mill is finished, take it out and filter it, put it in an oven for 6 hours at 80°C, take it out and grind it with a mortar for 30 minutes after it is completely dried, and then sieve it after grinding it into powder. After collecting and sieving, the powder was placed in a magnesia crucible for calcination at 800°C for 12 hours. After cooling, it was taken out and ground again for 30 minutes to form a powder. Part of the powder was sieved and collected as master powder. Repeat the ball milling work for another part of the powder, weigh 0.51g of alumina ...

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Abstract

The invention discloses an industrialized preparation method of a tantalum-aluminum-codoped lithium-lanthanum zirconate solid-state electrolyte. The product has a structure expression of Li6.4-XLa3Zr2-XTaXAl0.2O12, wherein X is 0.2 to 0.5. According to the method, a normal-pressure solid-phase sintering method is adopted, the preparation process is simple, used instruments are low in cost and easyin operation, and industrial production is facilitated; although the sintering time is relatively long, the final obtained product is high in density, good in experimental repeatability and high in ionic conductivity. Tantalum of a proper amount and aluminum of a proper amount are codoped, Al plays a role in stabilizing cubical-phase lithium-lanthanum zirconate, and Ta is used for effectively improving the electric conductivity of the lithium-lanthanum zirconate.

Description

technical field [0001] The invention relates to the field of preparation of solid electrolyte materials, in particular to an industrialized preparation method of a tantalum-aluminum co-doped lithium lanthanum zirconate solid electrolyte. Background technique [0002] Compared with other types of batteries, rechargeable lithium-ion batteries have higher output voltage and energy storage density, and are also more environmentally friendly, and are widely used in portable electronic equipment and electronic vehicles. At present, commercial lithium-ion batteries generally use liquid electrolytes. Although liquid electrolytes have high lithium-ion conductivity, they have shortcomings such as easy leakage, easy corrosion, and easy decomposition at high temperatures, which make them prone to safety hazards such as spontaneous combustion or explosion. The reaction produces lithium dendrites, which limits its large-scale application and use in the field of chemical energy storage. C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G35/00
CPCC01G35/006C01P2002/72C01P2004/03C01P2006/40
Inventor 尹延谋李明刘耀春
Owner 淮安新能源材料技术研究院
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