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Solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film and its preparation

A technology of lithium lanthanum zirconium oxide ceramics and electrolyte film, which is applied in electrolytes, circuits, electrical components, etc., can solve the problems of low lithium ion conductivity, high grain boundary impedance, poor surface compatibility, etc., and achieves broad application prospects and solutions. The effect of high brittleness and excellent flexibility

Active Publication Date: 2021-01-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects of complex process, high energy consumption, poor flexibility, high grain boundary impedance, poor surface compatibility and low lithium ion conductivity in the prior art, and provide a simple process, low cost and good flexibility. , solid-state LLZO ceramic nanofiber electrolyte film with small grain boundary resistance, good interface compatibility and high lithium ion conductivity, which is flexible and densely aligned and its preparation method

Method used

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  • Solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film and its preparation
  • Solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film and its preparation

Examples

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Embodiment 1

[0034] A method for preparing a solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film, the specific steps are:

[0035] (1) Configure a precursor solution consisting of a lithium source, a lanthanum source, a zirconium source, a polymer, and a solvent: Dissolve the polymer polyvinylpyrrolidone (Aladdin, molecular weight 1,300,000) in ethanol as a solvent at 28°C Stir for 40 minutes, then sequentially add lithium source lithium chloride, lanthanum source lanthanum chloride, and zirconium source zirconium oxychloride and stir for 120 minutes to prepare a precursor solution, in which the lithium source, lanthanum source, zirconium source, polymer polymer The mol ratio of substance and solvent is 7: 3: 2: 0.01: 1000;

[0036] (2) Prepare the precursor fiber film by electrospinning the above precursor solution, apply a constant temperature thermal field of 60°C in the spinning interval and control the temperature of the metal drum receiving device to -10°C duri...

Embodiment 2

[0039] A method for preparing a solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film, the specific steps are:

[0040] (1) Configure a precursor solution consisting of a lithium source, a lanthanum source, a zirconium source, a high molecular polymer and a solvent: the high molecular polymer polyvinyl butyral (Aladdin, molecular weight 170,000-250,000) Dissolve in solvent ethanol and stir for 80 minutes, then add lithium chloride source lithium, lanthanum source lanthanum chloride and zirconium source zirconium acetate in sequence and stir for 120 minutes to prepare a precursor solution, wherein lithium source, lanthanum source, zirconium source, high The molar ratio of molecular polymer to solvent is 7:3:2:0.09:1120;

[0041] (2) Prepare the precursor fiber film by electrospinning the above precursor solution, apply a constant temperature thermal field of 30°C in the spinning interval during electrospinning and control the temperature of the metal drum r...

Embodiment 3

[0044] A method for preparing a solid lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film, the specific steps are:

[0045] (1) Configure a precursor solution consisting of lithium source, lanthanum source, zirconium source, polymer and solvent: dissolve the polymer polyvinylidene fluoride (Alpha Aesar, molecular weight 570,000) in Stir in the solvent N, N-dimethylformamide for 60 minutes, then add lithium source lithium nitrate, lanthanum source lanthanum nitrate and zirconium source zirconium nitrate in sequence and stir for 60 minutes to prepare a precursor solution, wherein the solution contains lithium source, lanthanum source, The molar ratio of zirconium source, polymer and solvent is 3.5: 1.5: 1: 0.01: 500;

[0046] (2) Prepare the precursor fiber film by electrospinning the above precursor solution, apply a constant temperature thermal field of 30°C in the spinning interval and control the temperature of the metal drum receiving device to 0°C during e...

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Abstract

The invention provides a solid-state lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film and a production method thereof. The production method of the solid-state lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film comprises the following steps: 1, preparing a precursor solution, wherein the precursor solution is composed of a lithium source, a lanthanum source, azirconium source, a high-molecular polymer and a solvent; 2, electrospinning the precursor solution to obtain a precursor fiber film, applying a 20-80 DEG C constant temperature heat field in a spinning interval during the electrospinning, and controlling the temperature of a receiving device to be -10-30 DEG C and the rotating speed of the receiving device to be 50-100 n / min; and 3, calcining the precursor fiber film in an air atmosphere to obtain the solid-state lithium lanthanum zirconium oxide ceramic nanofiber electrolyte film. The solid-state LLZO ceramic nanofiber electrolyte film produced in the invention has an excellent flexibility, is a nanoscale continuously orientated fiber, and facilitates the migration of lithium ions, so the electric conductivity of particles is improved,thereby the film has very high practical use values, and can effectively meet practical requirements of a lithium ion battery in various applications.

Description

technical field [0001] The invention belongs to the field of new energy materials and technologies, and relates to a solid lithium lanthanum zirconium oxide (LLZO) ceramic nanofiber electrolyte film with flexible and dense alignment and a preparation method thereof, which can be used in the technical fields of all-solid lithium batteries and flexible lithium batteries, especially The invention relates to a method for preparing a solid electrolyte film by electrospinning. Background technique [0002] Currently, most commercial lithium batteries use organic liquid electrolytes. First of all, this type of electrolyte has safety problems such as easy leakage, flammability, and explosion, and it needs to be tightly packaged to ensure that the liquid electrolyte does not leak; second, the liquid electrolyte is easy to chemically react with the electrode, resulting in damage to the electrode structure and short circuit of the battery. Thirdly, the mass of the organic liquid elect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/0525D01F9/08
CPCD01F9/08H01M10/0525H01M10/0562H01M2300/0071Y02E60/10
Inventor 闫建华赵云丁彬俞建勇
Owner DONGHUA UNIV