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Preparation method for all-solid-state lithium ion electrolyte material Li7La3Zr2O12

An electrolyte material, lithium ion technology, applied in electrolytes, circuits, electrical components, etc., can solve the problems of easy mixing of molten salt into powder, reduce battery manufacturing costs, and require high-temperature sintering, so as to speed up ion transfer and reduce The effect of production cost and short calcination time

Inactive Publication Date: 2016-03-16
QINGDAO NENGXUN NEW ENERGY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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] The prior art reports a molten salt method for preparing 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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  • Preparation method for all-solid-state lithium ion electrolyte material Li7La3Zr2O12
  • Preparation method for all-solid-state lithium ion electrolyte material Li7La3Zr2O12
  • Preparation method for all-solid-state lithium ion electrolyte material Li7La3Zr2O12

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Experimental program
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Effect test

Embodiment 1

[0042] First, weigh lithium nitrate LiNO 3 10.33g, lithium hydroxide LiOH6.27g, dilanthanum trioxide La 2 o 3 3.66g, zirconium dioxide ZrO 2 1.83g. Then pour it into an agate mortar and grind it thoroughly 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 after 60 minutes, and calcined at this temperature for 5 hours. After the calcination, it was naturally lowered to room temperature in an argon atmosphere. Finally, the product was taken out, washed three times by centrifugation with deionized water, and dried under vacuum at 120° C. for 12 hours.

Embodiment 2

[0044] First, weigh lithium nitrate LiNO 3 6.89g, lithium hydroxide LiOH4.18g, dilanthanum trioxide La 2 o 3 2.44g, zirconium dioxide ZrO 2 1.22g. Then pour it into an agate mortar and grind it thoroughly 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 800°C after 60 minutes, and calcined at this temperature for 5 hours. After the calcination, it was naturally lowered to room temperature in an argon atmosphere. Finally, the product was taken out, washed three times by centrifugation with deionized water, and dried under vacuum at 120° C. for 12 hours.

Embodiment 3

[0046] First, weigh lithium nitrate LiNO 3 6.89g, lithium hydroxide LiOH4.18g, dilanthanum trioxide La 2 o 3 2.44g, zirconium dioxide ZrO 2 1.22g. Then pour it into an agate mortar and grind it thoroughly 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 ignite and calcinate, the furnace temperature rises to 700°C after 60 minutes, and calcines at this temperature for 5 hours. After the calcination, it was naturally lowered to room temperature in an argon atmosphere. Finally, the product was taken out, washed three times by centrifugation with deionized water, and dried under vacuum at 80° C. for 12 hours.

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Abstract

The invention discloses a preparation method for an all-solid-state lithium ion electrolyte material Li7La3Zr2O12. The preparation method comprises the following steps: (1) taking LiNO3 and LiOH as fused salt and a lithium source, and mixing and grinding LiNO3, LiOH, La2O3 and ZrO2; and (2) performing calcining on the grinded mixture in an inert atmosphere at the temperature of 700-900 DEG C for 3-5 hours, and then naturally cooling to the room temperature to obtain the all-solid-state lithium battery ion material Li7La3Zr2O12. The preparation method provided by the invention is short in calcining time, low in temperature, and simple in operation without introducing non-reactant foreign matters; and the product has a nanosheet laminated structure and a high specific surface, so that the ionic conductance at the normal temperature is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to an all-solid lithium ion electrolyte material Li 7 La 3 Zr 2 o 12 method of preparation. 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 fundamentally guarantee the...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0071Y02E60/10
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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