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Sintering method for reducing lithium ion loss of solid-state lithium ion electrolyte material Li7La3Zr2O12

A technology of electrolyte material and sintering method, which is applied to circuits, electrical components, secondary batteries, etc., can solve the problems of reducing battery manufacturing cost, high temperature sintering and high energy consumption, and mixing molten salt into powder, etc., so as to reduce production costs and reduce Calcination temperature, the effect of shortening the reaction period

Inactive Publication Date: 2016-03-23
QINGDAO NENGXUN NEW ENERGY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Third, some solid electrolytes are not sensitive to moisture and can maintain good chemical stability in the air for a long time. Therefore, the whole process of manufacturing solid-state batteries does not necessarily require the protection of an inert atmosphere, which will reduce the manufacturing cost of batteries to a certain extent.
Although its preparation method reduces the synthesis steps, it still inevitably requires high-temperature sintering and high-energy ball milling.
[0008] In Chinese Patent Publication No. CN103496740A, a kind of molten salt method is reported to prepare Li 7 La 3 Zr 2 o 12 The method of electrolyte powder, which uses KCl and LiCl as molten salt, although the sintering temperature can be appropriately reduced, but the molten salt is easily mixed into the powder after sintering, which is difficult to wash off, resulting in low product purity

Method used

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  • Sintering method for reducing lithium ion loss of solid-state lithium ion electrolyte material Li7La3Zr2O12

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh lithium carbonate Li 2 CO 3 3.70g, lithium nitrate LiNO 3 10.33g, lithium hydroxide LiOH6.27g, dilanthanum trioxide La 2 o 3 35.75g, zirconium dioxide ZrO 2 17.87g, and then pour the weighed raw materials into an agate mortar and grind them fully for 15 minutes to mix the raw materials evenly, and then transfer the ground powder to a magnesia crucible. The crucible was placed in a tube furnace, and high-purity argon gas was introduced slowly for 10 minutes to remove the air in the tube. Then ignited and calcined, the furnace temperature was raised to 750°C at a speed of 30°C / min, and calcined at this temperature for 3 hours. After the calcination, the temperature was naturally cooled to room temperature in an argon atmosphere.

Embodiment 2

[0024] Weigh lithium carbonate Li 2 CO 3 2.10g, lithium nitrate LiNO 3 5.76g, lithium hydroxide LiOH4.0g, dilanthanum trioxide La 2 o 3 21.23g, zirconium dioxide ZrO 2 10.61g, then pour the weighed raw materials into an agate mortar and grind them fully for 15 minutes to mix the raw materials evenly, then transfer the ground powder to a magnesia crucible. The crucible was placed in a tube furnace, and high-purity argon gas was introduced slowly for 10 minutes to remove the air in the tube. Then ignited and calcined, the furnace temperature was raised to 850°C at a rate of 30°C / min, and calcined at this temperature for 2 hours. After the calcination, the temperature was naturally cooled to room temperature in an argon atmosphere.

Embodiment 3

[0026] Weigh lithium carbonate Li 2 CO 3 3.70g, lithium nitrate LiNO 3 10.33g, lithium hydroxide LiOH6.27g, dilanthanum trioxide La2 o 3 35.75g, zirconium dioxide ZrO 2 17.87g, and then pour the weighed raw materials into an agate mortar and grind them fully for 15 minutes to mix the raw materials evenly, and then transfer the ground powder to a magnesia crucible. The crucible was placed in a tube furnace, and high-purity argon gas was introduced slowly for 10 minutes to remove the air in the tube. Then ignited and calcined, the furnace temperature was raised to 900°C at a rate of 20°C / min, and calcined at this temperature for 4 hours. After the calcination, the temperature was naturally cooled to room temperature in an argon atmosphere.

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Abstract

The present invention discloses a sintering method for reducing lithium ion loss of a solid-state lithium ion electrolyte material Li7La3Zr2O12. The method comprises a step of carrying out mixed sintering on lithium sources, La2O3 and ZrO2. The method is characterized in that the lithium sources are Li2CO3, LiNO3 and LiOH, and a sintering temperature of the method is 750-900 DEG C, wherein a mass ratio of Li2CO3 to LiNO3 to LiOH is 1:(2-3):(1-2). The sintering method disclosed by the present invention is low in burning temperature, is simple to operate, avoids introduction of non-reaction-product impurities, which is caused by high-temperature burnout, and can reach ion conductivity of 2.23*10-4S / cm under the normal temperature.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a lithium ion electrolyte material that reduces the 7 La 3 Zr 2 o 12 Sintering method for loss of lithium ions. Background technique [0002] In recent years, serious safety accidents have occurred in large-capacity lithium-ion batteries in the auxiliary power supply of electric vehicles and aircrafts. The cause of these problems is related to the use of flammable organic solvents in lithium-ion batteries. Although measures such as adding flame retardants, using high-temperature-resistant ceramic diaphragms, surface modification of positive and negative materials, optimizing battery structure design, optimizing BMS, coating phase-change flame-retardant materials on the outer surface of batteries, and improving cooling systems can achieve considerable To a certain extent, the safety of existing lithium-ion batteries can be improved, but these measures cannot fund...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/04H01M10/0525
CPCH01M10/04H01M10/0525H01M10/0562Y02E60/10Y02P70/50
Inventor 林展刘培杨李全国高学会刘磊许阳阳
Owner QINGDAO NENGXUN NEW ENERGY TECH CO LTD
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