Preparation method of NASICON-type lithium ion solid electrolyte

A solid electrolyte, lithium ion technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, electrolyte immobilization/gelation, etc., can solve the problems of low conductivity, high conductivity of solid electrolyte, complicated preparation process, etc. The effect of uniform and fine grains, improvement of sinterability and relative density, and improvement of ionic conductivity

Active Publication Date: 2014-05-28
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above defects or improvement needs of the prior art, the present invention provides a preparation method of a NASICON type lithium-ion solid electrolyte, which can effectively solve the problems of lo...

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  • Preparation method of NASICON-type lithium ion solid electrolyte
  • Preparation method of NASICON-type lithium ion solid electrolyte
  • Preparation method of NASICON-type lithium ion solid electrolyte

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preparation example Construction

[0027] The preparation method of the NASICON type lithium ion solid electrolyte of the embodiment of the present invention comprises the following steps:

[0028] (1) Weigh lithium nitrate, aluminum nitrate, tetrabutyl titanate and ammonium dihydrogen phosphate according to the stoichiometric ratio.

[0029] (2) Dissolving citric acid in water to obtain a citric acid solution with a concentration of 1-2 mol / L.

[0030] (3) Dissolve lithium nitrate and aluminum nitrate in citric acid solution, stir to form a transparent and uniform nitrate mixed solution. Wherein, the ratio of the amount of citric acid to the metal cation in the nitrate mixed solution is 1:1.

[0031] (4) Prepare absolute ethanol with the same volume as the water in step (2), dissolve tetrabutyl titanate in absolute ethanol, stir to make it clear and transparent, and form an alcohol solution of tetrabutyl titanate.

[0032] (5) In a constant temperature environment, slowly add the tetrabutyl titanate alcohol ...

Embodiment 1

[0041] The preparation method of NASICON type lithium ion solid electrolyte comprises the steps:

[0042](1) Weigh lithium nitrate, aluminum nitrate, tetrabutyl titanate and ammonium dihydrogen phosphate according to the stoichiometric ratio.

[0043] (2) Dissolve citric acid in water to obtain a citric acid solution with a concentration of 1mol / L.

[0044] (3) Dissolve lithium nitrate and aluminum nitrate in citric acid solution, stir to form a transparent and uniform nitrate mixed solution. Wherein, the ratio of the amount of citric acid to the metal cation in the nitrate mixed solution is 1:1.

[0045] (4) Prepare absolute ethanol with the same volume as the water in step (2), dissolve tetrabutyl titanate in absolute ethanol, stir to make it clear and transparent, and form an alcohol solution of tetrabutyl titanate.

[0046] (5) In a constant temperature environment of 80°C, slowly add the tetrabutyl titanate alcohol solution prepared in step (4) into the nitrate mixed so...

Embodiment 2

[0054] The preparation method of NASICON type lithium ion solid electrolyte comprises the steps:

[0055] (1) Weigh lithium nitrate, aluminum nitrate, tetrabutyl titanate and ammonium dihydrogen phosphate according to the stoichiometric ratio.

[0056] (2) Dissolve citric acid in water to obtain a citric acid solution with a concentration of 1mol / L.

[0057] (3) Dissolve lithium nitrate and aluminum nitrate in citric acid solution, stir to form a transparent and uniform nitrate mixed solution. Wherein, the ratio of the amount of citric acid to the metal cation in the nitrate mixed solution is 1:1.

[0058] (4) Prepare absolute ethanol with the same volume as the water in step (2), dissolve tetrabutyl titanate in absolute ethanol, stir to make it clear and transparent, and form an alcohol solution of tetrabutyl titanate.

[0059] (5) In a constant temperature environment of 80°C, slowly add the tetrabutyl titanate alcohol solution prepared in step (4) into the nitrate mixed s...

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Abstract

The invention discloses a preparation method of an NASICON-type lithium ion solid electrolyte. The method comprises the following steps: dissolving lithium nitrate and aluminum nitrate in a citric acid solution, and stirring to form a transparent and uniform nitrate mixed solution; dissolving tetrabutyl titanate in anhydrous ethanol, and stirring to form an alcoholic solution of tetrabutyl titanate; slowly adding the alcoholic solution of tetrabutyl titanate to the nitrate mixed solution, and stirring to a transparent mixed solution; dissolving ammonium biphosphate in water to obtain a saturated aqueous solution of ammonium biphosphate, adding the saturated aqueous solution of ammonium biphosphate to the transparent mixed solution in a dropwise manner, and stirring to obtain an emulsion; adjusting the pH value of the emulsion, and drying the emulsion to obtain an xerogel; carrying out heat treatment of the xerogel, and grinding the obtained xerogel to form fine powder which is precursor powder; and compacting the precursor powder to form a green body, and sintering to obtain NASICON-type lithium ion solid electrolyte slices. The method has the advantages of low energy consumption, simplicity, easy implementation, and convenience for large-scale industrialized production, and the obtained solid electrolyte has a high conductivity.

Description

technical field [0001] The invention belongs to the field of solid electrolyte preparation, and more specifically relates to a preparation method of a NASICON type lithium ion solid electrolyte. Background technique [0002] The increasingly prominent energy and environmental issues and the wide application of electronic products have promoted the development and research of new high-capacity, green, safe, lightweight and portable energy storage devices. Secondary batteries have become a golden key to solve the energy environment and meet the urgent needs of electronic products. Among many secondary batteries, rechargeable lithium-ion batteries have become the new favorite of many researchers because of their high specific capacity and excellent cycle stability. The research and development of a new generation of high-capacity lithium-ion batteries such as lithium-sulfur batteries and lithium-air batteries has made it possible for electric vehicles to replace fuel-driven ve...

Claims

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Application Information

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IPC IPC(8): H01M10/058H01M10/0562
CPCH01M10/058H01M2300/0085Y02E60/10Y02P70/50
Inventor 朱文贾迎宾李镜人赵旭东
Owner HUAZHONG UNIV OF SCI & TECH
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