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Preparation method of lithium iron borate

A technology of lithium iron borate and iron nitrate, applied in borates, chemical instruments and methods, boron compounds, etc., can solve problems such as easy absorption of moisture and oxygen, large specific surface area of ​​products, and decline in product performance, and achieve capacity decay Low efficiency, good stability and small particle size

Active Publication Date: 2018-11-06
临汾市中贝新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the conventional method is to mix borate, iron salt and lithium salt and then calcine. The biggest problem in the solid phase reaction is uneven mixing, and the obtained product has a large specific surface area, which is easy to absorb moisture and oxygen, resulting in a decline in product performance.

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  • Preparation method of lithium iron borate
  • Preparation method of lithium iron borate
  • Preparation method of lithium iron borate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of preparation method of lithium iron borate, it is the following steps:

[0031] (1) Mix the lithium borohydride solution and the ferric nitrate solution into a sealed high-pressure reactor, stir and react for 50 minutes at a temperature of 235°C and a pressure of 3 atmospheres, then release the pressure, and pour the derived gas with ferrous hydroxide Slurry absorption, then add aluminum citrate, stir and mix evenly, and then spray dry to obtain dry material;

[0032] (2) Sinter the dry material obtained in step (1) under an inert atmosphere. The calcination is divided into a heating section, a heat preservation section and a cooling section. The maintenance temperature in the section is 705°C, the residence time in the holding section is 17 hours, the cooling rate in the cooling section is 110°C / h, and the calcined material is obtained by cooling to a temperature below 60°C;

[0033] (3) The obtained calcined material is subjected to airflow crushing through ...

Embodiment 2

[0042] A kind of preparation method of lithium iron borate, it is the following steps:

[0043] (1) Mix the lithium borohydride solution and the ferric nitrate solution into a sealed high-pressure reactor, stir and react for 50 minutes at a temperature of 240°C and a pressure of 3.5 atmospheres, and then release the pressure. Slurry absorption, then add aluminum citrate, stir and mix evenly, and then spray dry to obtain dry material;

[0044] (2) The dry material obtained in step (1) is sintered under an inert atmosphere. The calcination is divided into a heating section, a heat preservation section and a cooling section. The maintenance temperature in the section is 706°C, the residence time in the holding section is 18 hours, the cooling rate in the cooling section is 107°C / h, and the calcined material is obtained by cooling to a temperature below 60°C;

[0045] (3) The obtained calcined material is subjected to airflow crushing through nitrogen gas, then sieved to remove iro...

Embodiment 3

[0054] A kind of preparation method of lithium iron borate, it is the following steps:

[0055] (1) Mix lithium borohydride solution and ferric nitrate solution into a sealed high-pressure reaction kettle, stir and react for 45 minutes at a temperature of 240°C and a pressure of 3.5 atmospheres, and then release the pressure. Slurry absorption, then add aluminum citrate, stir and mix evenly, and then spray dry to obtain dry material;

[0056] (2) Sinter the dry material obtained in step (1) under an inert atmosphere. The calcination is divided into a heating section, a heat preservation section and a cooling section. The maintenance temperature in the section is 703°C, the residence time in the holding section is 19 hours, the cooling rate in the cooling section is 107°C / h, and the calcined material is obtained by cooling to a temperature below 60°C;

[0057] (3) The obtained calcined material is subjected to airflow crushing through nitrogen gas, then sieved to remove iron, ...

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Abstract

The invention discloses a preparation method of lithium iron borate. The preparation method comprises the following steps: mixing a lithium borohydride solution with a ferric nitrate solution and pouring a mixed solution into a sealed high-pressure reactor, carrying out hydrothermal reaction and then decompressing; absorbing the exported gas with ferric hydroxide slurry, adding aluminum citrate, uniformly stirring and mixing and then carrying out spray drying to obtain a dry material; sintering the dry material in an inert atmosphere, cooling to a temperature below 60 DEG C and discharging toobtain a calcined material; carrying out fluid energy milling on the obtained calcined material by using nitrogen, screening, removing iron and carrying out vacuum packaging to obtain a cathode material of the lithium iron borate. According to the preparation method of the lithium iron borate, disclosed by the invention, amorphous lithium iron borate is prepared by using the hydrothermal method, is coated with alumina citrate and is then calcined at high temperature to obtain the lithium iron borate coated with alumina and carbon; the lithium iron borate has the advantages of small primary particle size, good stability and good electrochemical property.

Description

technical field [0001] The invention relates to a preparation method of lithium iron borate, which belongs to the field of new energy battery materials. Background technique [0002] Lithium iron borate (LiFeBO3) is used as a cathode material for high-capacity lithium batteries. The theoretical specific capacity is 220mAh / g, and the theoretical specific capacity of lithium iron phosphate is only 170mAh / g. It has better conductivity and a very small volume change rate (~2%). In terms of structure, the molar mass of borate (BO3) is smaller than (PO4) (58.8<95), and the structure of lithium iron borate can provide lithium ion conductivity and electronic conductivity at the same time. Preparation of this material requires great care, as the electrochemical performance of the material deteriorates rapidly upon contact with moisture. [0003] At present, the conventional method is to mix borate, iron salt and lithium salt and then calcine. The biggest problem in the solid phas...

Claims

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Application Information

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IPC IPC(8): C01B35/12
CPCC01B35/128C01P2006/11C01P2006/12C01P2006/80
Inventor 方嘉城
Owner 临汾市中贝新材料有限公司
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