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A method of treating inorganic solid electrolyte with phosphorus-containing organic matter

A technology of solid electrolyte and organic matter, which is applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, 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: 2021-05-18
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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  • A method of treating inorganic solid electrolyte with phosphorus-containing organic matter
  • A method of treating inorganic solid electrolyte with phosphorus-containing organic matter
  • A method of treating inorganic solid electrolyte with phosphorus-containing organic matter

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 to be fired into LLZTO ceramic sheets, and cooled naturally ....

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 in a water bath at 80 ° C and evaporate to dryness, and place the material obtained after evaporation to dryness in a In a Furnace, calcined at 750 °C for 2 h, and cooled naturally to obtain the treated LLZTO. The obtained treated 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 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 wit...

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Abstract

The invention provides a method for treating inorganic solid electrolyte with phosphorus-containing organic matter. The method utilizes the phosphorus element in the organic compound to treat the inorganic solid electrolyte in a non-aqueous system, completely avoiding the adverse effects of water on the inorganic solid electrolyte, and making the phosphorus-containing organic matter in the inorganic The surface of the solid electrolyte is evenly distributed, and during the subsequent high-temperature calcination treatment, the phosphorus element reacts with the residual lithium on the surface at high temperature to consume the residual lithium on the surface. By adjusting the concentration of phosphorus-containing organic matter, the residual lithium on the surface of the solid electrolyte can be reduced while maintaining the structural stability of the inorganic solid electrolyte and excellent lithium ion conductivity. The phosphorus-containing organic compound utilized in the invention has wide sources and low cost; the liquid phase method is adopted, the conditions are mild, the process is simple and effective, and industrial production is easy. This method is the first application of phosphorus-containing organic compounds on solid electrolytes, and has broad application prospects in inorganic solid electrolyte materials.

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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Patent Type & Authority Patents(China)
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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