Al<3+> doped and modified LGPS type lithium ion solid electrolyte and preparation method thereof

A solid electrolyte, lithium ion technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., can solve the problems of high raw material cost, poor interface stability, complex synthesis process, etc. , the effect of easy industrialization

CN113823830AActive Publication Date: 2021-12-21SICHUAN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2021-12-21

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Abstract

The invention discloses an Al<3+> doped and modified LGPS type lithium ion solid electrolyte and a preparation method thereof. The general formula of the solid electrolyte is Li10.35Ge1.35-0.75xAlxP1.65S12, wherein x is more than or equal to 0.05 and less than or equal to 0.20 in the general formula. The solid electrolyte is prepared by adopting a traditional solid phase process. The preparation method comprises the working procedures of batching, primary ball milling, compression molding, primary sintering, secondary ball milling, compression molding, secondary sintering, gold plating and the like. According to the Al<3+> doped and modified LGPS type lithium ion solid electrolyte provided by the invention, Al<3+> is doped in the Ge<4+> position in the LGPS structure, so that the LGPS type lithium ion solid electrolyte with excellent room-temperature lithium ion conductivity performance is obtained, and the room-temperature lithium ion conductivity can reach 22.1 mS / cm. The preparation method of the lithium ion solid electrolyte is stable and mature in process, the adopted raw materials are easy to obtain, and the lithium ion solid electrolyte has universality and industrial practicability and is easy to industrialize.
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Description

technical field

[0001] The invention belongs to the field of all-solid lithium ion batteries, relates to an LGPS type lithium ion solid electrolyte, in particular to an Al 3+ Doping modified LGPS type lithium ion solid state electrolyte and preparation method thereof. Background technique

[0002] Due to safety and energy density considerations, all-solid-state lithium-ion batteries have received more and more attention. On the one hand, all-solid-state lithium-ion batteries can fundamentally solve the flammable and explosive problems that liquid lithium-ion batteries cannot avoid due to the organic electrolyte; on the other hand, all-solid-state batteries can solve the problem that traditional liquid lithium-ion batteries are difficult to use metal Lithium is a difficult problem as a negative electrode material, and the wide electrochemical window can be adapted to the use of high potential positive electrode materials. The dense fast ion conductor electrolyte can effectiv...

Examples

Embodiment 1

[0029] The present embodiment prepares by general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Expressed Al 3+ The doped modified LGPS type lithium ion solid electrolyte, where x=0.05, specifically includes the following steps:

[0030] (1) Ingredients: Li 2 S, GeS 2 ,P 2 S 5 and Al 2 S 3 As raw material, according to the general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Determine the molar ratio to weigh the ingredients;

[0031] (2) Primary ball milling: Mix and dry-mill the raw materials prepared in step (1) until they are fully mixed and uniform to obtain primary ball milling powder, and use a mold to press the primary ball milling powder into a columnar disc for subsequent use;

[0032] (3) Primary sintering: crush the compacted disc green body in step (2) into pieces of appropriate size and place them in a quartz tube, vacuum-pack the quartz tube, and place the quartz tube with the sample in the muffle Sintering in the furnace at 580°C for 8h to...

Embodiment 2

[0037] The present embodiment prepares by general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Expressed Al 3+ The doped modified LGPS type lithium ion solid electrolyte, where x=0.10, specifically includes the following steps:

[0038] (1) Ingredients: Li 2 S, GeS 2 ,P 2 S 5 and Al 2 S 3 As raw material, according to the general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Determine the molar ratio to weigh the ingredients;

[0039] (2) Primary ball milling: Mix and dry-mill the raw materials prepared in step (1) until they are fully mixed and uniform to obtain primary ball milling powder, and use a mold to press the primary ball milling powder into a columnar disc for subsequent use;

[0040] (3) Primary sintering: crush the compacted disc green body in step (2) into pieces of appropriate size and place them in a quartz tube, vacuum-pack the quartz tube, and place the quartz tube with the sample in the muffle Sintering in the furnace at 580°C for 8h to...

Embodiment 3

[0045] The present embodiment prepares by general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Expressed Al 3+ The doped modified LGPS type lithium ion solid electrolyte, where x=0.20, specifically includes the following steps:

[0046] (1) Ingredients: Li 2 S, GeS 2 ,P 2 S 5 and Al 2 S 3 As raw material, according to the general formula Li 10.35 Ge 1.35-0.75x Al x P 1.65 S 12 Determine the molar ratio to weigh the ingredients;

[0047] (2) Primary ball milling: Mix and dry-mill the raw materials prepared in step (1) until they are fully mixed and uniform to obtain primary ball milling powder, and use a mold to press the primary ball milling powder into a columnar disc for subsequent use;

[0048] (3) Primary sintering: crush the compacted disc green body in step (2) into pieces of appropriate size and place them in a quartz tube, vacuum-pack the quartz tube, and place the quartz tube with the sample in the muffle Sintering in the furnace at 580°C for 8h to...