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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AI-Extracted 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 inven...

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Method used

[0071] (2) In the molding process of the present invention, heating and pressurization are adopted to promote the filling of ...

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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.

Application Domain

Secondary cells

Technology Topic

IonThermal treatment +10

Examples

Experimental program(6)
Comparison scheme(1)

Example Embodiment

[0050] Example 1

[0051] In the glove box, weigh out Li according to 75∶25 2 S and P 2 S 5 , Added to the container containing dehydrated tetrahydrofuran. Stir at 600 rpm for 48h. The resulting suspension was vacuum filtered. The obtained powder was precipitated and dried at 150°C and -0.1MPa for 2h. Put the obtained powder into a sealed ball mill tank, vacuum the ball mill tank, and ball mill for 3 hours at a rotation speed of 300 rpm. Take out the material in the glove box, heat treatment 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 put into 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 prepared solid electrolyte has an ionic conductivity of 1.3×10 at room temperature -3 S/cm.

Example Embodiment

[0053] Example 2

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

[0055] The electrolyte obtained above was put into 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 prepared solid electrolyte has an ionic conductivity of 6.2×10 at room temperature -3 S/cm.

Example Embodiment

[0056] Example 3

[0057] In the glove box, weigh Li according to 70:25 2 S, P 2 S 5 , Added to a container containing anhydrous acetonitrile. Stir at 1000 rpm for 36 hours. The resulting suspension was dried at 150°C and -0.1MPa for 12 hours. The obtained powder and the metering ratio of LiCl (Li 2 S: P 2 S 5 :LiCl=70:25:5) Put it into a sealed ball mill jar, evacuate the ball mill jar, and ball mill for 3 hours at 300 rpm. Take out the material in the glove box, heat treatment 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 the NMP sizing and apply it on the PET film, pass 5 sets of counter rolls (total length 0.6m) with a pitch of 30μm and a temperature of 150℃ at a speed of 10cm/min, and then peel off after vacuum drying at 80℃ for 1h. Sulfide electrolyte membrane. The prepared solid electrolyte has an ionic conductivity of 9.2×10 at room temperature -4 S/cm.

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PUM

Property	Measurement	Unit
Thickness	10.0 ~ 100.0	µm
Thickness	30.0	µm
Ionic conductivity	0.0013	s/cm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Polyarylether containing quaternary ammonium side group and its preparation method, and anion exchange membrane containing quaternary ammonium side group and its preparation method

ActiveCN103788365ALow water absorptionImprove ionic conductivitySolid electrolyte fuel cellsFuel cell detailsHalogenIon-exchange membranes

Owner:CHINA PETROLEUM & CHEM CORP +1

Polymer solid electrolyte, all-solid-state lithium battery and preparation method of all-solid-state lithium battery

PendingCN112701348AHigh bonding strengthImprove ionic conductivitySolid electrolytesSecondary cellsElectrically conductiveIn situ polymerization

Owner:SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA

Classification and recommendation of technical efficacy words

Improve ionic conductivity

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

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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