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High-ion-conductivity sulfide solid electrolyte based on wet ball milling and preparation method thereof

A technology of solid electrolyte and wet ball milling, which is applied in the direction of electrochemical generators, circuits, electrical components, etc., can solve the problems of reduced electrical conductivity, achieve the effects of eliminating grain boundary resistance, promoting synthesis, and promoting coupling reactions

Active Publication Date: 2019-06-14
NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention utilizes a solvent-promoted ball milling method to obtain a sulfide solid-state electrolyte of the target crystal form; the present invention solves the problem of a decrease in electrical conductivity caused by a pore structure inside the electrolyte after the solvent escapes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] In the glove box, weigh Li according to 75:25 2 S and P 2 S 5 , adding zirconia grinding balls according to the ball-to-material ratio of 20:1, and adding tetrahydrofuran after molecular sieve dehydration equivalent to 50% of the raw material mass. It is sealed in a high-tightness zirconia ball mill jar with an air nozzle. Put into ball mill, ball mill with the rotating speed of 500 rpm for 12 hours. The ball mill jar is connected to a vacuum pump, in which is connected a cold trap to recover the solvent. Put the ball mill jar into the heating jacket, control the temperature at 60°C, open the air nozzle, pump the air pressure inside the ball mill jar to -0.1MPa (relative air pressure), and dry for 4 hours. Close the gas nozzle again, keep the vacuum in the ball mill jar, and ball mill for 3 hours again at a speed of 300 rpm. The material was taken out from the glove box, and heat-treated at 150° C. for 4 hours under the protection of an inert atmosphere to obtain t...

Embodiment 2

[0063] In the glove box, weigh Li according to 70:29:1 2 S, P 2 S 5 and P 2 o 5 , adding zirconia grinding balls according to the ball-to-material ratio of 15:1, and adding anhydrous acetonitrile equivalent to 50% of the raw material mass. It is sealed in a high-tightness zirconia ball mill jar with an air nozzle. Put into ball mill, ball mill with the rotating speed of 600 rpm for 10 hours. The ball mill jar is connected to a vacuum pump, in which is connected a cold trap to recover the solvent. Put the ball mill jar into the heating jacket, control the temperature at 80°C, open the air nozzle, pump the air pressure inside the ball mill jar to -0.1MPa (relative air pressure), and dry for 4 hours. Close the air nozzle again, keep the air pressure in the ball mill jar, and ball mill for 3 hours again at a speed of 300 rpm. The material was taken out from the glove box, and heat-treated at 150° C. for 4 hours under the protection of an inert atmosphere to obtain the targe...

Embodiment 3

[0066] In the glove box, weigh Li according to 75:20:5 2 S, P 2 S 5 and LiI, adding zirconia grinding balls according to the ball-to-material ratio of 10:1, and adding tetrahydrofuran dehydrated by molecular sieves equivalent to 10% of the raw material mass. It is sealed in a high-tightness zirconia ball mill jar with an air nozzle. Put into ball mill, ball mill with the rotating speed of 600 rpm for 14 hours. The ball mill jar is connected to a vacuum pump, in which is connected a cold trap to recover the solvent. Put the ball mill jar into the heating jacket, control the temperature at 60°C, open the air nozzle, pump the air pressure inside the ball mill jar to -0.1MPa (relative air pressure), and dry for 3 hours. Close the air nozzle again, keep the air pressure in the ball mill jar, and ball mill for 3 hours again at a speed of 300 rpm. The material was taken out from the glove box, and heat-treated at 140° C. for 4 hours under the protection of an inert atmosphere to...

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Abstract

The invention discloses a high-ion-conductivity sulfide solid electrolyte based on wet ball milling and a preparation method thereof. The preparation method comprises the following steps: (1) adding raw materials at least comprising Li2S and P2S5, a grinding medium and a solvent into a ball milling tank for sealed ball milling to obtain a mixture a; (2) drying the mixture a under reduced pressure,sealing the ball milling tank under a reduced pressure state, and performing ball milling again to obtain a mixture b; (3) and taking out the mixture b from a glove box, and performing heat treatmentunder the protection of inert atmosphere to obtain the high-ion-conductivity sulfide solid electrolyte material. According to the invention, the porous structure introduced by solvent and crystallization solvent molecules in the obtained sulfide solid electrolyte is eliminated by secondary ball milling under reduced pressure after drying under reduced pressure, so that the high-ion-conductivity sulfide solid electrolyte is obtained. The invention further adopts a hot pressing or hot paired roller mode for molding, thereby enhancing the combination effect of the sulfide solid electrolyte and further improving the ionic conductivity.

Description

technical field [0001] The invention relates to the technical field of solid electrolytes, in particular to a high ion conductivity sulfide solid electrolyte based on wet ball milling and a preparation method thereof. Background technique [0002] The ever-increasing consumption of digital electronics and the emerging electric vehicle industry have put forward higher requirements for energy storage devices. Lithium secondary batteries have many advantages such as high energy density, excellent cycle performance, no memory effect and no environmental pollution, and are favored by the market. However, lithium-ion batteries using organic electrolytes are gradually failing in the face of the market's increasingly high requirements for safety, energy density, and cycle life. [0003] All-solid lithium secondary batteries using solid electrolytes have incomparable safety compared to liquid lithium secondary batteries, and are expected to completely eliminate potential safety haza...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCY02E60/10
Inventor 卢骋陈功田光磊佘圣贤
Owner NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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