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High-ion-conductivity sulfide solid electrolyte based on liquid phase method and preparation method thereof

A solid electrolyte, high-ion technology, applied in electrochemical generators, circuits, electrical components, etc., can solve problems such as the reduction of electrical conductivity, and achieve the effect of eliminating grain boundary resistance, improving electrolyte performance, and improving ionic conductivity.

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 the liquid phase method to obtain the sulfide solid electrolyte of the target crystal form; the present invention solves the problem that the electrical conductivity decreases due to the pore structure inside the electrolyte after the solvent escapes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] In the glove box, weigh Li according to 75:25 2 S and P 2 S 5 , into the vessel containing the dehydrated THF. Stir at 600 rpm for 48h. The resulting suspension was vacuum filtered. The obtained powder precipitate was dried at 150°C and -0.1MPa for 2h. The obtained powder was put into a sealed ball mill jar, and the ball mill jar was evacuated, and ball milled at a speed of 300 rpm for 3 hours. The material was taken out from the glove box, and heat-treated at 200° C. for 1 h under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.

[0052] The electrolyte obtained above was added to a mold, and hot-pressed at 100 MPa and 100° C. for 30 minutes to obtain a sulfide solid electrolyte sheet with a thickness of 30 μm. The ionic conductivity of the prepared solid electrolyte at room temperature is 1.3×10 -3 S / cm.

Embodiment 2

[0054] In the glove box, weigh Li according to 70:29 2 S, P 2 S 5 , into the vessel containing the dehydrated THF. Stir at 600 rpm for 24h. The obtained suspension was dried at 150°C and -0.1MPa for 12h. The obtained powder and the P of the metering ratio 2 o 5 (Li 2 S:P 2 S 5 :P 2 o 5 =70:29:1) into a sealed ball mill jar, and the ball mill jar was evacuated, and ball milled at a speed of 300 rpm for 3 hours. The material was taken out from the glove box, and heat-treated at 230° C. for 2 hours under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.

[0055] The electrolyte obtained above was added to a mold, and hot-pressed at 100 MPa and 100° C. for 30 minutes to obtain a sulfide solid electrolyte sheet with a thickness of 30 μm. The ionic conductivity of the prepared solid electrolyte at room temperature is 6.2×10 -3 S / cm.

Embodiment 3

[0057] In the glove box, weigh Li according to 70:25 2 S, P 2 S 5 , into a vessel containing anhydrous acetonitrile. Stir at 1000 rpm for 36h. The obtained suspension was dried at 150°C and -0.1MPa for 12h. The obtained powder and the LiCl (Li 2 S:P 2 S 5 : LiCl=70:25:5) into a sealed ball mill jar, and the ball mill jar was evacuated, and ball milled for 3 h at a speed of 300 rpm. The material was taken out from the glove box, and heat-treated at 260° C. for 1 h under the protection of an inert atmosphere to obtain the target sulfide solid electrolyte.

[0058] Add the obtained electrolyte to NMP slurry and apply it on the PET film, pass through 5 pairs of rollers (total length 0.6m) with a distance of 30 μm and a temperature of 150°C at a speed of 10cm / min, and peel off after vacuum drying at 80°C for 1 hour to obtain Sulfide electrolyte membrane. The ionic conductivity of the prepared solid electrolyte at room temperature is 9.2×10 -4 S / cm.

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Abstract

The invention discloses a high-ion-conductivity sulfide solid electrolyte based on a liquid phase method and a preparation method thereof. The preparation method comprises the following steps: (1) adding raw materials at least comprising Li2S and P2S5 and a solvent into a stirring container, stirring, performing vacuum filtration, and drying under reduced pressure to obtain a mixture a; (2) filling the mixture a in the step (1) into a ball milling tank, vacuumizing, and performing ball milling to obtain a mixture b; (3) and taking out the mixture b in the step (2) from a glove box, and performing heat treatment under 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 solidelectrolyte 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 a liquid phase method 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] Inorganic solid electrolytes have the advantages of non-flammability, wide electrochemical stability window, and large shear modulus, and have the advantages of safety and service life that org...

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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