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Method for rapidly preparing spinel type Li4Ti5O12 lithium titanate material at low temperature

A spinel type, lithium titanate technology, applied in titanate, alkali metal titanate, chemical instruments and methods, etc., can solve the problems of low preparation efficiency and lithium loss, and achieve uniform particle size and high rate performance. , the effect of reducing energy consumption

Pending Publication Date: 2021-02-19
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to aim at spinel type Li 4 Ti 5 o 12 Problems such as low preparation efficiency and lithium loss in the existing preparation technology provide a method for preparing spinel-type Li at low temperature. 4 Ti 5 o 12 Lithium titanate material method

Method used

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  • Method for rapidly preparing spinel type Li4Ti5O12 lithium titanate material at low temperature
  • Method for rapidly preparing spinel type Li4Ti5O12 lithium titanate material at low temperature
  • Method for rapidly preparing spinel type Li4Ti5O12 lithium titanate material at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] This example uses the solid oxide mixing method combined with the flash firing process to prepare spinel Li 4 Ti 5 o 12 Lithium titanate material, the specific preparation process is as follows:

[0030] Weigh 6.44g of lithium carbonate powder, 17.40g of titanium dioxide powder, and 50mL of ethanol and mix them in a 250mL zirconia ball mill jar, add 120g of zirconia grinding balls with a diameter of 3mm, and reinforce the lid; place the packaged ball mill jar on a ball mill for ball milling, set The rotation speed is 100r / min, and the ball milling time is set to 12h; the obtained mixed solution is dried in an oven after removing the solvent, and the oven temperature is set to 60°C, and then the dried material is fully ground and sieved to obtain the flash precursor powder.

[0031] Put the flash-fired precursor powder into a cuboid cemented carbide mold, and carry out compression molding. The molding pressure is 200 MPa, and the holding time is 2 minutes; 4×4mm 2 , ...

Embodiment 2

[0035] In this example, spinel Li was prepared by hydrothermal method combined with flash firing process. 4 Ti 5 o 12 Lithium titanate material, the specific preparation process is as follows:

[0036] Dissolve 10.0g of butyl titanate in 60.0mL of ethanol to obtain a titanium source solution, and at the same time dissolve 1.62g of lithium nitrate in 60.0mL of water to obtain a lithium source solution; fully stir the titanium source solution and lithium source solution to obtain a mixed solution; mix The liquid is placed in a hydrothermal kettle, and the hydrothermal kettle containing the mixed solution is placed in an oven for hydrothermal reaction. The filling degree in the hydrothermal kettle is 60%, and the reaction temperature of the hydrothermal reaction is 180°C. The reaction time of the hydrothermal reaction at the reaction temperature is 24 hours; the hydrothermal reaction product is cooled to room temperature, dried, ground, and sieved to obtain the flash precursor ...

Embodiment 3

[0041] This example utilizes sol-gel method combined with flash firing process to prepare spinel Li 4 Ti 5 o 12 The specific preparation process of lithium titanate material is as follows:

[0042] Dissolve 2.64g of lithium acetate and 38.4g of citric acid in 75.0mL of ethanol and 5.0mL of deionized water to prepare a lithium source solution; dissolve 17.0g of butyl titanate in 100mL of ethanol to prepare a titanium source solution; vigorously stir the titanium Source solution, lithium source solution was slowly added dropwise to titanium source solution, the reaction temperature was controlled to maintain at room temperature, and a transparent sol was obtained by continuous stirring, and then aged for 24 hours to obtain a milky white wet gel; the wet gel was placed in an oven and heated at 120 Dry at a constant temperature for 18 hours at °C to obtain a xerogel, and then grind and sieve the xerogel to obtain a flash precursor powder.

[0043] Put the flash-fired precursor ...

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Abstract

The invention provides a method for rapidly preparing a spinel type Li4Ti5O12 lithium titanate material at a low temperature, and belongs to the technical field of lithium titanate preparation. The preparation method comprises the following steps of: (1) preparing flash burning precursor powder of Li4Ti5O12 by using a solid oxide mixing method, a hydrothermal method or a sol-gel method; (2) putting the flash burning precursor powder prepared in the step (1) into a mold, carrying out compression molding, demolding, and carrying out isostatic cool pressing treatment to obtain a final flash burning precursor biscuit; and (3) applying direct current to the two ends of the flash burning precursor biscuit, heating the flash burning precursor biscuit in a protective atmosphere until the flash burning is finished, starting flash burning when flash occurs, controlling the current density, controlling the flash burning for a period of time in a constant current state, stopping heating after theflash burning is completed, cooling to room temperature to obtain a Li4Ti5O12 sintered body, and crushing to obtain a spinel type Li4Ti5O12 lithium titanate powder product. According to the invention,the preparation of the precursor powder and the flash burning technology are combined, the temperature and time required by preparation are reduced, and the preparation energy consumption is saved.

Description

technical field [0001] The invention belongs to the technical field of preparation of lithium titanate, in particular to a method for rapidly preparing spinel-type Li at low temperature. 4 Ti 5 o 12 Lithium titanate material method. Background technique [0002] Spinel Li 4 Ti 5 o 12 Lithium titanate has become a widely used lithium battery material due to its good cycle performance, outstanding safety performance, very small volume change and low cost. Spinel lithium titanate (Li 4 Ti 5 o 12 ) traditional preparation methods mainly include high-temperature solid-state reaction method, hydrothermal method and sol-gel method. [0003] In the traditional high-temperature solid-state reaction preparation method, the synthesis process temperature is high, the sintering time is long, the energy consumption is large, the production efficiency is low, the particle size distribution of the product is not easy to control, and the uniformity, consistency and reproducibility a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00H01M4/485H01M10/052
CPCC01G23/005H01M4/485H01M10/052C01P2002/72C01P2006/40Y02E60/10
Inventor 徐晨刘方明白彬
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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