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Li7La3Zr2O12 ion conductor ceramic fiber and preparation method thereof

A technology of lithium lanthanum zirconium oxide and ion conductors, which is applied in the direction of inorganic raw materials such as artificial filaments, can solve the problems of ion conductor ceramic fiber chemical structure, shape size and electrical conductivity differences, complex preparation process, poor stability, etc., to achieve compensation Li-ion conductivity, enhanced rate performance, and reduced clogging rate

Active Publication Date: 2017-05-17
QINGTAO KUNSHAN ENERGY DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of ionic ceramic fibers using these processes is relatively complicated and the cost is high, and the chemical structure, shape, size and electrical conductivity of the ionic conductor ceramic fibers obtained by the above processes are also different, and the stability is poor.

Method used

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  • Li7La3Zr2O12 ion conductor ceramic fiber and preparation method thereof
  • Li7La3Zr2O12 ion conductor ceramic fiber and preparation method thereof
  • Li7La3Zr2O12 ion conductor ceramic fiber and preparation method thereof

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preparation example Construction

[0028] The present invention also provides a preparation method of lithium lanthanum zirconium oxide ion conductor ceramic fiber, comprising the following steps:

[0029] 1) lithium carbonate, lanthanum oxide, zirconyl nitrate, nitric acid solution and absolute ethanol are mixed and heated to obtain a mixed solution;

[0030] 2) Mix citric acid and ethylene glycol with the mixed solution obtained in step 1) to obtain a lithium lanthanum zirconium oxygen precursor, wherein the molar ratio of lithium carbonate, lanthanum oxide, zirconyl nitrate, ethylene glycol and citric acid is 7 :3:4:28:14, stirring the lithium lanthanum zirconium oxygen precursor at a constant temperature to obtain a precursor sol;

[0031] 3) mixing and stirring the water-soluble polymer with the precursor sol obtained in the step 2) to obtain the spinning sol;

[0032] 4) Calcining the spinning sol obtained in step 3) after spinning to obtain ion conductor ceramic fibers.

[0033] The present invention d...

Embodiment 1

[0047] Weigh lithium carbonate (Li 2 CO 3 )5.69g, lanthanum oxide (La 2 o 3 ) 9.77g, zirconium oxynitrate (ZrO(NO 3 ) 2 )9.25g, lithium carbonate (Li 2 CO 3 ), lanthanum oxide (La 2 o 3 ) was dissolved in 80g concentration of 15% dilute nitric acid solution, zirconium oxynitrate (ZrO(NO 3 ) 2 ) was dissolved in 20g of absolute ethanol, wherein Lithium Carbonate weighed 10% more to compensate for the volatilization of lithium under high temperature.

[0048] Mix the above-mentioned nitric acid solution dissolved in lithium carbonate and lanthanum oxide with absolute ethanol dissolved in zirconium oxynitrate, and stir in a constant temperature water bath environment at 50°C, then add 53.80g of citric acid and 8.69g of ethylene glycol, and keep the temperature constant Stirred for 12h to obtain a sol.

[0049] 50 g of PVP solution with a mass concentration of 10% was weighed and mixed with the obtained sol, and stirred thoroughly for 24 hours. The obtained sol was use...

Embodiment 2

[0053] Weigh lithium carbonate (Li 2 CO 3 )5.69g, lanthanum oxide (La 2 o 3 ) 9.77g, zirconium oxynitrate (ZrO(NO 3 ) 2 )9.25g, lithium carbonate (Li 2 CO 3 ), lanthanum oxide (La 2 o 3 ) was dissolved in 50g concentration of 20% dilute nitric acid solution, zirconium oxynitrate (ZrO(NO 3 ) 2 ) was dissolved in 40g absolute ethanol, wherein Lithium Carbonate weighed 10% more to compensate for the volatilization of lithium under high temperature.

[0054] Mix the above-mentioned nitric acid solution dissolved in lithium carbonate and lanthanum oxide with absolute ethanol dissolved in zirconium oxynitrate, and stir in a constant temperature water bath environment at 80°C, then add 53.80g of citric acid and 8.69g of ethylene glycol, and keep the temperature constant Stirred for 24h to obtain a sol.

[0055] Weigh 45g of PVP solution with a mass concentration of 10%, mix with the obtained sol, and stir thoroughly for 48h. The obtained sol was used for air spinning at a...

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Abstract

The invention discloses Li7La3Zr2O12 ion conductor ceramic fiber. The material has the chemical composition of Li7La3Zr2O12, has the ion conductor ceramic fiber length of 1-2.5 mu m, the diameter of 80-120 nm and the lithium ion conductivity of 1.5*10<-4> S / cm-6*10<-3> S / cm. The invention further provides a method for preparing the ion conductor ceramic fiber. Lithium carbonate, lanthanum oxide, zirconyl nitrate, a nitric acid solution and absolute ethyl alcohol are mixed, heated and then mixed with citric acid and ethylene glycol, and the mixture is stirred at the constant temperature, and precursor sol is obtained; spinning sol is obtained by mixing a water-soluble polymer and the obtained precursor sol, spinning and calcination are performed sequentially, and ion conductor ceramic fiber with stable morphology and size is obtained. The method can improve the lithium ion conductivity significantly, adopts a simple process, is low in cost, has low requirements for equipment and environment and is suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of inorganic materials, in particular to a lithium lanthanum zirconium oxide ion conductor ceramic fiber and a preparation method thereof. Background technique [0002] At this stage, lithium-ion batteries have direct conduction between positive and negative electrodes and short-circuit phenomenon, and the safety performance cannot be guaranteed. The reason is that most of the electrolytes are liquid, and a diaphragm is set in the middle of the electrolyte to separate the positive and negative electrodes of the battery and prevent them from being connected directly. The normal passage of lithium ions requires a certain porosity in the separator, and the heating of the battery will cause the shrinkage of the organic separator, causing the positive and negative electrodes to be directly connected to form a short circuit; the solid electrolyte is not volatile and generally non-flammable, so the choice of solid ...

Claims

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Application Information

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IPC IPC(8): C04B35/50D01F9/08
CPCC04B35/50C04B35/62231C04B2235/3203C04B2235/3244
Inventor 冯玉川李峥何泓材何朝凌杨帆南策文
Owner QINGTAO KUNSHAN ENERGY DEV CO LTD
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