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LLZO preparation method, thermal cell quasi-solid electrolyte, and preparation method thereof

An electrolyte, quasi-solid-state technology, applied in the field of material chemistry, can solve the problems of short calcination time, high corrosion of equipment, no large-scale production, etc., and achieve good thermal stability, high ion mobility, and small grain boundary resistance.

Active Publication Date: 2019-06-14
SHANGHAI INST OF SPACE POWER SOURCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN105489930A adopts a kind of molten salt method to prepare LLZO, and this method calcining temperature is lower, and calcining time is shorter, and the LLZO electrical conductivity that makes is higher (1.6×10 -4 S / cm), but due to the use of LiCl-KCl eutectic salt, it is highly corrosive to equipment at high temperatures (700-800 ° C), and there is no possibility of large-scale production at present.

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  • LLZO preparation method, thermal cell quasi-solid electrolyte, and preparation method thereof
  • LLZO preparation method, thermal cell quasi-solid electrolyte, and preparation method thereof

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preparation example Construction

[0028] The preparation method of quasi-solid electrolyte for thermal battery of the present invention comprises:

[0029] Step 1, in an environment with a dew point lower than -40°C, the La 2 o 3 Baking at 800℃~1000℃ for 12h~15h to remove La(OH) 3 Impurities, the Li 2 CO 3 , ZrO 2 、H 2 C 2 o 4 Place the eutectic salt with alkali metal halides in a blast drying oven, dry for 2 hours to 4 hours, and the drying temperature is 120 ° C to 150 ° C;

[0030] Preferably, the alkali metal halide eutectic salt is a LiF-LiCl-LiBr system (the mass percentage of LiF in the system is 8-11%, the mass percentage of LiCl is 21-23%, and the mass percentage of LiBr 67-70%), LiCl-LiBr-KBr system (the mass percentage of LiCl in the system is 11-13%, the mass percentage of LiBr is 35-38%, and the mass percentage of KBr is 50-53%) or LiCl-KCl system (the mass percentage of LiCl in the system is 44-46%, the mass percentage of KCl is 54-56%);

[0031] Step 2, according to the component conte...

Embodiment 1

[0037] The amount of each raw material is calculated according to the ratio of each component in the target product quasi-solid electrolyte. In this example, in an environment with a dew point lower than -40°C, the La 2 o 3 Placed at 900°C for 12 hours to remove La(OH) 3 Impurities, weigh 98g of La after heat treatment 2 o 3 , 57g Li 2 CO 3 (10% excess), 49g ZrO 2 , 306 g H 2 C 2 o 4 (accounting for La 2 o 3 , Li 2 CO 3 , ZrO 2 and H 2 C 2 o 4 60% of the total mass of the four materials) and 30g LiF-LiCl-LiBr system eutectic salt (accounting for 15% of the quasi-solid electrolyte quality), the Li 2 CO 3 , ZrO 2 、H 2 C 2 o 4 The eutectic salt of LiF-LiCl-LiBr system was placed in a blast drying oven, and dried for 2 hours at a drying temperature of 120°C. 98g La 2 o 3 , 57g Li 2 CO 3 , 49 g ZrO 2 and 306g H 2 C 2 o 4 Put it into an agate mortar, grind it evenly, put it into a stainless steel tank, bake it at 1200°C for 2 hours, cool it down to roo...

Embodiment 2

[0041] The amount of each raw material is calculated according to the ratio of each component in the target product quasi-solid electrolyte. In this example, in an environment with a dew point lower than -40°C, the La 2 o 3 Placed at 900°C for 12 hours to remove La(OH) 3 Impurities, weigh 98g of La after heat treatment 2 o 3 , 57g Li 2 CO 3 (10% excess), 49g ZrO 2 , 408 g H 2 C 2 o 4 (accounting for La 2 o 3 , Li 2 CO 3 , ZrO 2 and H 2 C 2 o 4 67% of the total mass of the four materials) and 9g LiCl-KCl system eutectic salt (accounting for 5% of the quasi-solid electrolyte quality), the Li 2 CO 3 , ZrO 2 、H 2 C 2 o 4 Place the eutectic salt with LiCl-KCl system in a forced air drying oven and dry for 2 hours at a drying temperature of 120°C. 98g La 2 o 3 , 57g Li 2 CO 3 , 49 g ZrO 2 and 408g H 2 C 2 o 4 Put it into an agate mortar, grind it evenly, put it into a stainless steel tank, bake it at 1200°C for 2 hours, cool it down to room temperature...

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Abstract

The invention relates to a LLZO preparation method, a thermal cell quasi-solid electrolyte, and a preparation method thereof. The preparation method of the quasi-solid electrolyte comprises followingsteps: raw materials including Li2CO3, La2O3, ZrO2, H2C2O4, and an alkali metal halide are subjected to purification treatment, the needed Li2CO3, La2O3, H2C2O4, and ZrO2 are weighed, are grinded to be uniform, and are introduced into a sealed stainless steel tank for roasting at 1200 DEG C, natural cooling is carried out, an obtained product is subjected to ball milling to be uniform so as to obtain the lithium lanthanum zirconium oxygen solid state electrolyte (Li7La3Zr2O12, LLZO); the LLZO and an alkali metal halide co-molten salt are mixed again, the temperature is increased to 400 to 500DEG C under protection of argon gas rapidly, repeat vacuum pumping and slow pressurizing are carried out so that infiltration of the co-molten salt into the porous LLZO is realized, natural cooling iscarried out, and an obtained product is subjected to ball milling so as to obtain the thermal cell quasi-solid electrolyte. The prepared thermal cell quasi-solid electrolyte is low in crystal boundary resistance, and high in ion mobility, and heat stability.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a preparation method of LLZO, a quasi-solid electrolyte for thermal batteries and a preparation method thereof. Background technique [0002] At present, thermal batteries used as missile-borne power sources use alkali metal halide eutectic salts as electrolytes, which are flowable liquids above the eutectic point. Although the flow inhibitor MgO will be added to the electrolyte to form the spacer powder when preparing the thermal battery, with the continuous improvement of the performance of the weapon system, the requirements for the battery to resist the mechanical environment are getting higher and higher. However, there is still a risk of electrolyte spillage, causing a short circuit in the battery. The use of solid electrolyte materials with strong thermal stability, wide electrochemical window, and non-melting within the operating temperature range of thermal batteries t...

Claims

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Application Information

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IPC IPC(8): C01G25/00H01M6/22H01M6/36
Inventor 叶丹宏张维义强杉杉郑侠李长江胡华荣越云博刘凯特
Owner SHANGHAI INST OF SPACE POWER SOURCES
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