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Method for treating inorganic solid electrolyte by using phosphorus-containing organic substance

A technology of solid electrolyte and organic matter, applied in non-aqueous electrolyte batteries, electrolyte battery manufacturing, circuits, etc., can solve the problems of large-scale, low-cost operations, limitations, etc., and achieve excellent lithium ion conductivity, mild conditions, and The effect of maintaining structural stability

Active Publication Date: 2019-11-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods are limited by expensive experimental equipment and cannot achieve large-scale, low-cost operations

Method used

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  • Method for treating inorganic solid electrolyte by using phosphorus-containing organic substance
  • Method for treating inorganic solid electrolyte by using phosphorus-containing organic substance
  • Method for treating inorganic solid electrolyte by using phosphorus-containing organic substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Preparation of LLZTO

[0042] 4.88gLa 2 o 3 , 2.16gZrO 2 , 0.55gTa 2 o 5 , 3gLi 2 CO 3 Place in a 500ml agate ball mill jar, mill at 400r / min for 12h, put the milled product in a muffle furnace, and calcinate at 900°C for 10h. Obtain garnet-type inorganic solid-state electrolyte Li 6.75 La 3 Zr 1.75 Ta 0.25 o 12 (LLZTO) calcined powder.

[0043] 2. Dealing with LLZTO

[0044] Disperse 1g of LLZTO calcined powder into 100ml of methanol, add 0.1g of hexachlorotrimeric phosphazene, stir for 2h, place in a water bath at 80°C and evaporate to dryness, and place the material obtained after evaporation in a muffle furnace at 750°C Calcined for 2 hours and cooled naturally to obtain the treated LLZTO. The processed LLZTO material and untreated LLZTO calcined powder were respectively pressed into tablets in a 12mm mold under a pressure of 20MPa, and the pressed tablets were calcined at 1120°C for 16h, fired into LLZTO ceramic sheets, and cooled naturally . The...

Embodiment 2

[0046] Disperse 1 g of the LLZTO calcined powder prepared in Example 1 into 100 ml of methanol, add 5%, 10%, and 20% of the mass of hexachlorotrimeric phosphazene respectively, stir for 2 hours, and evaporate to dryness in a water bath at 80°C , the material obtained after evaporation to dryness was placed in a muffle furnace, calcined at 750°C for 2h, and cooled naturally to obtain the treated LLZTO. The obtained processed LLZTO material was pressed into a tablet in a 12 mm mold under a pressure of 20 MPa, and the pressed sheet was calcined at 1120° C. for 16 hours to be fired into a LLZTO ceramic sheet and cooled naturally. The cooled LLZTO ceramic flakes were ground into powder for characterization. The obtained materials were respectively dispersed in water at a ratio of 1:10, stirred ultrasonically, left to stand for 30 minutes, and the pH value was tested. The results are shown in Table 1. It can be seen from the test results that the method of the invention effectively...

Embodiment 3

[0050] Disperse 1 g of the LLZTO calcined powder prepared in Example 1 into 100 ml of methanol, add 0.04 g of hexachlorotrimeric phosphazene, stir for 2 h, place it in a water bath at 80 ° C and evaporate to dryness, and place the material obtained after evaporation to dryness in a horse In a Furnace, calcined at 750°C for 2h, and cooled naturally to obtain the treated LLZTO. The obtained treated LLZTO material was pressed into a tablet in a 12mm mold under a pressure of 20MPa, and the pressed sheet was calcined at 1120°C for 16h to be fired into a LLZTO ceramic sheet and cooled naturally. The cooled LLZTO ceramic flakes were ground into powder for characterization. The processed LLZTO and the untreated LLZTO were subjected to micro-Raman test, the test wavelength was 532nm, and the test results were as follows image 3 As shown, the Li contained in the treated LLZTO 2 CO 3 significantly decreased, indicating that during the calcination process, the phosphorus reacted with ...

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Abstract

The invention provides a method for treating an inorganic solid electrolyte by using a phosphorus-containing organic substance. According to the method, an inorganic solid electrolyte is treated in anon-aqueous system by using phosphorus in an organic compound, so that side effects of water on the inorganic solid electrolyte are completely avoided, the phosphorus-containing organic substance is uniformly distributed on the surface of the inorganic solid electrolyte through a liquid-phase mixing or in-situ polymerization scheme; and the phosphorus reacts with residual lithium on the surface athigh temperature to consume the residual lithium on the surface during subsequent high-temperature calcination. The structure stability and excellent lithium ion conductivity of the inorganic solid electrolyte are kept through adjusting the concentration of the phosphorus-containing organic substance, and meanwhile, the residual lithium on the surface of the solid electrolyte is reduced. The phosphorus-containing organic compound utilized in the method is wide in source and low in cost. By adopting a liquid phase method, the method provided by the invention is mild in condition, simple and effective in process and easy for industrialized production. The method is a first application of the phosphorus-containing organic substance in the solid electrolyte and has a broad application prospect in the inorganic solid electrolyte material.

Description

technical field [0001] The invention belongs to the field of lithium-ion battery electrolytes, and in particular relates to a method for treating inorganic solid-state electrolytes with phosphorus-containing organic matter. Background technique [0002] Electric vehicles are an important area of ​​national planning and development. Safety concerns are one of the obstacles to the development of electric vehicles. An important part of the safety issue of electric vehicles is the lithium-ion battery electrolyte. Most of the existing lithium-ion battery electrolytes are liquid electrolytes or polymer electrolytes. When the battery temperature control system fails and the temperature rises, this type of electrolyte will burn and catch fire, which will promote the oxygen evolution of the positive electrode material, trigger a chain reaction, and cause the electric vehicle to explode. [0003] Inorganic solid-state electrolytes can solve the safety problems caused by existing lit...

Claims

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Application Information

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IPC IPC(8): H01M10/058H01M10/0562
CPCH01M10/0562H01M10/058Y02E60/10Y02P70/50
Inventor 曹安民陶现森万立骏
Owner INST OF CHEM CHINESE ACAD OF SCI
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