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Sulfide solid electrolyte, preparation method thereof and all-solid-state lithium secondary battery

A technology of solid electrolyte and sulfide, which is applied in the manufacture of solid electrolyte, non-aqueous electrolyte storage battery, and electrolyte storage battery, etc. It can solve problems such as easy deliquescence, poor air stability, and increased battery preparation and use costs.

Active Publication Date: 2018-07-06
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most sulfide solid electrolytes have poor air stability and are prone to deliquescence and hydrogen sulfide gas after contact with air. Therefore, the use process must be carried out under airtight conditions, which increases the cost of battery preparation and use.

Method used

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  • Sulfide solid electrolyte, preparation method thereof and all-solid-state lithium secondary battery
  • Sulfide solid electrolyte, preparation method thereof and all-solid-state lithium secondary battery
  • Sulfide solid electrolyte, preparation method thereof and all-solid-state lithium secondary battery

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preparation example Construction

[0046] The present invention also provides a preparation method of a sulfide solid electrolyte, comprising the following steps:

[0047] A) will Li 2 S and P 2 S 5 Mixing and grinding with metal oxides to obtain raw materials; the metal oxides are zinc oxide or antimony oxide;

[0048] B) under the condition of inert gas, heat treatment is carried out to described initial material, obtain the sulfide lithium ion solid electrolyte as shown in formula (I) or (II);

[0049] Li 3+3x P 1-x Zn x S 4-x o x Formula I; Li 3 P 1-x Sb x S 4-2.5x o 2.5x Formula II;

[0050] Among them, 0.01≤x≤0.05.

[0051] In the present invention, the milling is preferably carried out under an inert gas, preferably nitrogen or argon.

[0052] In the present invention, since the valences of Zn and Sb are different, Li 2 S and P 2 S 5 There are also differences in the dosage, specifically,

[0053] When the metal oxide is zinc oxide:

[0054] Since Zn has a valence of +2, but the P e...

Embodiment 1

[0072] Under the protection of argon atmosphere, Li with a purity of more than 99% 2 S, P 2 S 5 , ZnO according to the molar ratio of Li 2 S:P 2 S 5 :ZnO=303:99:2 Weighing, grinding and mixing uniformly at 200rpm under the condition of water content less than 10ppm, high-energy ball milling under the condition of 10:1 ball-to-material ratio to obtain the primary powder after 9 hours, take out the primary powder and grind After being fine and uniform, use 10MPa pressure to press the tablet to obtain the flake-like raw material, and put the flake-like raw material into the sintering mold. Heat the sintering mold equipped with the above-mentioned flaky raw material to 150°C at a heating rate of 1°C / min, keep it warm for 1h, cool down to room temperature with the furnace, take out the flaky sintered product under the condition that the water content is less than 100ppm, and grind it evenly to obtain The powder is a lithium-ion solid electrolyte material for an all-solid-state...

Embodiment 2

[0075] Under the protection of argon atmosphere, Li with a purity of more than 99% 2 S, P 2 S 5 , ZnO according to the molar ratio of Li 2 S:P 2 S 5:ZnO=306:98:4 Weighing, grinding and mixing uniformly at a speed of 500rpm under the condition of water content less than 10ppm, high-energy ball milling under the condition of 45:1 ball-to-material ratio to obtain the primary powder after 13.5h, take out the primary powder After grinding evenly, use 10MPa pressure to press the tablet to obtain the flake raw material, and put the flake raw material into the sintering mold. Heat the sintering mold equipped with the above flake raw material to 250°C at a heating rate of 2°C / min, keep it warm for 2h, cool down to room temperature with the furnace, take out the flake sintered product under the condition that the water content is less than 100ppm, and grind it evenly to obtain The powder is a lithium-ion solid electrolyte material for an all-solid-state lithium secondary battery, t...

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Abstract

The invention provides a sulfide solid electrolyte which has a chemical formula shown in formula I or formula II: Li3+3xP1-xZnxS4-xOx (formula I) and Li3P1-xSbxS4-2.5xO2.5x (formula II), wherein x isgrater than or equal to 0.01 and less than or equal to 0.05. According to the invention, a certain amount of ZnO or Sb2O5 is used for double-doping modification of a sulfide solid electrolyte materialLi3PS4 to not only improve air stability of the modified sulfide solid electrolyte, but also benefit to improvement of electrical conductivity of lithium ions. The invention also provides a preparation method of the sulfide solid electrolyte and an all-solid-state lithium secondary battery.

Description

technical field [0001] The invention belongs to the technical field of lithium batteries, and in particular relates to a sulfide solid electrolyte, a preparation method thereof and an all-solid lithium secondary battery. Background technique [0002] Energy crisis and environmental pollution have increasingly become prominent problems restricting the sustainable development of human society, and it is becoming more and more urgent to develop and utilize green and clean energy. Electrochemical energy storage technology is crucial to the utilization of intermittent clean renewable energy such as solar energy and wind energy, and is also the core of zero-emission pure electric vehicles. Therefore, it is of great significance to develop energy storage devices with high efficiency, safety, large capacity, long service life, and stable energy release during use. Lithium-ion batteries are regarded as one of the most competitive electrochemical energy storage technologies due to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/058H01M10/0525C01G30/00C01G9/00
CPCC01G9/006C01G30/002H01M10/0525H01M10/0562H01M10/058H01M2300/0068Y02E60/10Y02P70/50
Inventor 陈少杰刘高瞻谢东九许晓雄
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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