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Solid electrolyte material and preparation method thereof

A technology of solid electrolyte and solid phase reaction, applied in circuits, electrical components, secondary batteries, etc., can solve problems such as long-term stability and cycleability, poor chemical stability, etc.

Active Publication Date: 2014-01-01
陕西泽邦环境科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems of poor chemical stability caused by easy hydrolysis and oxidation of existing solid electrolyte materials, long-term stability and cycle performance are difficult to guarantee, the present invention provides a solid electrolyte material and its preparation method to meet its Application in all-solid-state lithium batteries

Method used

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Experimental program
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Effect test

Embodiment 1

[0030] According to the general formula: 0.5Li 2 S-0.5P 2 S 5 -0.5 Ge 0.35 Ga 0.05 Se 0.60 , weighing the stoichiometric Li 2 S (purity ≥ 99.0%), P 2 S 5 (purity ≥ 99.0%) and Ge 0.35 Ga 0.05 Se 0.60 (purity ≥ 99.0%);

[0031] Put the above materials into a quartz glass tube, vacuumize it so that the vacuum degree is less than 10 -2 After Pa, it is sealed with hydrogen-oxygen flame;

[0032] Heating to 950°C for 24 hours of solid phase reaction;

[0033] Immediately after the reaction was completed, it was taken out and cooled to room temperature with ice water;

[0034] Open the tube to take out the powder, and perform high-energy ball milling under an argon atmosphere for 12 hours to obtain the solid electrolyte powder material.

[0035] Press the pressure of 10MPa into a cylinder with a diameter of 10mm and a thickness of 1mm, and then press a thin layer of indium film on both surfaces as a conductive electrode, and evaluate the conductivity on an electrochemic...

Embodiment 2

[0039] According to the general formula: 0.5Li 2 S-0.8P 2 S 5 -0.2 Ge 0.38 Ga 0.02 S 0.60 , weighing the stoichiometric Li 2 S (purity ≥ 99.0%), P 2 S 5 (purity ≥ 99.0%) and Ge 0.38 Ga 0.02 S 0.60 (purity ≥ 99.0%);

[0040] Put the above materials into a quartz glass tube, vacuumize it so that the vacuum degree is less than 10 -2 After Pa, it is sealed with hydrogen-oxygen flame;

[0041] Heating to 750°C for a solid phase reaction for 20 hours;

[0042] Immediately after the reaction was completed, it was taken out and cooled to room temperature with ice water;

[0043] Open the tube to take out the powder, and perform high-energy ball milling in an argon atmosphere for 8 hours to obtain the solid electrolyte powder material.

[0044] Press the pressure of 10MPa into a cylinder with a diameter of 10mm and a thickness of 1mm, and then press a thin layer of indium film on both surfaces as a conductive electrode, and evaluate the conductivity on an electrochemical ...

Embodiment 3

[0047] According to the general formula: 0.5Li 2 S-0.2P 2 S 5 -0.8 Ge 0.38 Ga 0.02 Se 0.60 , weighing the stoichiometric Li 2 S (purity ≥ 99.0%), sublimed sulfur (purity ≥ 99.999%), red phosphorus powder (purity ≥ 99.0%) and Ge 0.38 Ga 0.02 Se 0.60 (purity ≥ 99.0%);

[0048] Put the above materials into a quartz glass tube, vacuumize it so that the vacuum degree is less than 10 -2 After Pa, it is sealed with hydrogen-oxygen flame;

[0049] Heating to 850°C for a solid phase reaction for 12 hours;

[0050] Immediately after the reaction was completed, it was taken out and cooled to room temperature with ice water;

[0051] Open the tube to take out the powder, and perform high-energy ball milling under an argon atmosphere for 4 hours to obtain the solid electrolyte powder material.

[0052] Press the pressure of 10MPa into a cylinder with a diameter of 10mm and a thickness of 1mm, and then press a thin layer of indium film on both surfaces as a conductive electrode,...

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Abstract

The invention discloses a solid electrolyte material and a preparation method thereof, and the general formula of composition of the material is 0.5Li2S-xP2S5-(1-x) Ge0.4-yGayQ0.60, wherein Q is S or Se, x is not less than 0.1 and not more than 0.9 and y is not less than 0 and not more than 0.1. The preparation method of the material comprises the following steps: weighing Li2S, P2S5 and Ge0.4-yGayQ0.60 in the chemical metering ratio according to the general formula; loading into a closed container, vacuumizing and then packaging; heating to 500-1000 DEG C and performing solid-phase reaction for 5-36 hours; quenching to room temperature; and performing high-energy ball milling. The solid electrolyte material provided by the invention is high in ionic conductivity at room temperature and low in electron conductivity, has a wider electrochemical stability window and better chemical stability and can be used as a relatively ideal electrolyte material for a solid-state lithium-ion battery.

Description

technical field [0001] The invention relates to a solid electrolyte material and a preparation method thereof, in particular, the invention relates to a solid electrolyte material applicable to an all-solid lithium battery and a preparation method thereof. Background technique [0002] At present, most of the electrolytes used in lithium batteries contain volatile and flammable organic solvents, and the organic electrolytes in batteries can easily lead to serious fires and electrolyte leakage. The most effective way to overcome these problems and create a reliable battery is to replace the flammable liquid electrolyte with a nonflammable solid electrolyte. Compared with traditional liquid electrolyte batteries, all-solid lithium batteries not only have higher energy, but also avoid the corrosion of containers by liquid electrolytes such as acid and alkali, and have the advantages of no leakage, long storage life, and easy miniaturization. The wide range of operating tempera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562
CPCY02E60/12Y02E60/10
Inventor 黄富强刘战强
Owner 陕西泽邦环境科技有限公司