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Organic-inorganic composite solid electrolyte membrane and preparation method and application thereof

A technology of solid-state electrolyte membrane and solid-state electrolyte, applied in the direction of electrolyte immobilization/gelation, circuits, electrical components, etc., can solve the problem of low ion conductance, achieve high ion conductivity, wide electrochemical window, improve lithium ion The effect of migration number

Active Publication Date: 2022-01-28
郑州中科新兴产业技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problem of low ion conductance of organic-inorganic composite solid-state electrolyte membranes in the prior art, the present invention provides a preparation method of organic-inorganic composite solid-state electrolyte membranes, by adding modified active inorganic fillers to PEO-based polymer electrolytes to destroy the polymerization The original highly ordered structure of the material reduces its crystallinity and improves the ionic conductivity of the electrolyte membrane. At the same time, after the surface of the active inorganic filler is modified with ZiF material, it has a larger specific surface area and enhances the interaction between the inorganic material and the organic material PEO. Interface compatibility, effectively reducing interface internal resistance

Method used

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  • Organic-inorganic composite solid electrolyte membrane and preparation method and application thereof
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  • Organic-inorganic composite solid electrolyte membrane and preparation method and application thereof

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Effect test

Embodiment 1

[0028] A method for preparing an organic-inorganic composite solid electrolyte membrane, comprising the following steps:

[0029] (1) Preparation of LLZO@ZiF-67 powder: Add 0.5g PVP to 50mL methanol solution, stir well, then add 0.5g LLZO powder, stir at room temperature for 1 hour, add 2.3284g (0.008mol) Co(NO 3 ) 2 ·6H 2 O, to obtain solution A; then add 2.6272g (0.032mol) dimethylimidazole to 50mL methanol solution, stir at room temperature for 3h to obtain solution B; slowly add solution B to solution A, continue stirring at room temperature for 12h, and then Centrifuge at 1 / min for 5 minutes, wash the obtained purple precipitate with methanol three times, transfer the washed purple precipitate to a blast oven, and dry at 60°C for 6 hours to finally obtain purple LLZO@ZiF-67 powder;

[0030] (2) Prepare 20wt% LLZO@ZiF-67 / PEO / LiTFSI composite solid electrolyte membrane slurry: Weigh 0.88g PEO and 0.3824gLiTFSI into 22mL acetonitrile solution, keep stirring, then add 0.252...

Embodiment 2

[0034] A method for preparing an organic-inorganic composite solid electrolyte membrane, comprising the following steps:

[0035] (1) Preparation of LLZO@ZiF-67 powder: same as step (1) in Example 1;

[0036] (2) Prepare 10wt% LLZO@ZiF-67 / PEO / LiTFSI composite solid electrolyte membrane slurry: Weigh 0.88g PEO and 0.3824gLiTFSI into 20mL acetonitrile solution, keep stirring, then add 0.1262g LLZO@ZiF-67(LLZO The amount of @ZiF-67 added is 10wt% of the sum of the mass of PEO and LiTFSI) as a filling material, and stirred at room temperature for 12 hours to form a uniform composite electrolyte membrane slurry;

[0037] (3) Preparation of 10wt% LLZO@ZiF-67 / PEO / LiTFSI composite solid electrolyte membrane: In a glove box with water and oxygen content less than 0.1ppm, the composite electrolyte membrane slurry is poured into polytetrafluoroethylene by solution casting method In the template, it was left to stand in the glove box for 48 hours, then transferred to a vacuum drying oven...

Embodiment 3

[0039] A method for preparing an organic-inorganic composite solid electrolyte membrane, comprising the following steps:

[0040] (1) Preparation of LLZO@ZiF-67 powder: same as step (1) in Example 1;

[0041] (2) Prepare 30wt% LLZO@ZiF-67 / PEO / LiTFSI composite solid electrolyte membrane slurry: Weigh 0.88g PEO and 0.3824gLiTFSI into 24mL acetonitrile solution, keep stirring, then add 0.3787g LLZO@ZiF-67(LLZO The amount of @ZiF-67 added is 30wt% of the sum of the mass of PEO and LiTFSI) as a filling material, and stirred at room temperature for 12 hours to form a uniform composite electrolyte membrane slurry;

[0042] (3) Preparation of 30wt% LLZO@ZiF-67 / PEO / LiTFSI composite solid electrolyte membrane: In a glove box with water and oxygen content less than 0.1ppm, the composite electrolyte membrane slurry is poured into polytetrafluoroethylene by solution casting method In the template, it was left to stand in the glove box for 48 hours, then transferred to a vacuum drying oven...

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Abstract

The invention discloses an organic-inorganic composite solid-state electrolyte membrane and a preparation method thereof. The solid-state electrolyte membrane is mainly composed of PEO, LiTFSI and ZiF modified active inorganic filler, and the preparation method of the organic-inorganic composite solid-state electrolyte membrane comprises the following steps: synthesizing a ZiF material on the surface of the active inorganic filler in situ through an in-situ growth reaction; carrying out centrifuging, washing and drying to obtain modified active inorganic filler powder; uniformly mixing the modified active inorganic filler powder with PEO and LiTFSI to form composite electrolyte membrane slurry; and pouring the composite electrolyte membrane slurry into a mold by adopting a solution casting method to prepare the organic-inorganic composite solid electrolyte membrane. The ionic conductivity of the prepared electrolyte membrane can reach 7 times of that of a PEO / LiTFSI electrolyte membrane, and the problem that the ionic conductivity of an existing PEO-based solid electrolyte is lower at room temperature is effectively solved. The method is simple in process, high in preparation yield, low in cost and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium batteries, and in particular relates to an organic-inorganic composite solid-state electrolyte membrane and its preparation method and application. Background technique [0002] With the rapid development of electric vehicles, lithium metal batteries with high energy density have received more and more attention. However, in traditional liquid electrolytes, the unstable deposition process of lithium metal and the growth of lithium dendrites can lead to short-circuit combustion or even explosion of the battery, which seriously hinders the development of lithium metal batteries. The use of solid electrolytes with good safety performance and no potential electrolyte leakage can fundamentally solve the safety problem of lithium metal batteries. [0003] As the core of all-solid-state batteries, solid-state electrolytes are the top priority of the entire solid-state battery research and development. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0565H01M10/0525H01M10/42
CPCH01M10/0525H01M10/0565H01M10/4235H01M2300/0085Y02E60/10
Inventor 刘艳侠杨晓宇杨宝玉刘目浩王爽李德照柴丰涛高文超
Owner 郑州中科新兴产业技术研究院