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Preparation method of composite lithium iron borate

A technology of lithium iron borate and boric acid, applied in the field of new energy battery materials, can solve the problems of easy absorption of moisture and oxygen, large specific surface area of ​​products, and reduced product performance, etc., to achieve good dispersion, reduce powder internal resistance, and reduce BET Effect

Inactive Publication Date: 2020-08-18
蒋达金
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The products obtained by the current conventional methods have a large specific surface area, which is easy to absorb moisture and oxygen, resulting in a decrease in product performance.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of composite lithium iron borate, which is the following steps:

[0044] (1) Boric acid is dissolved in ethanol to obtain boric acid-ethanol solution, iron stearate is dissolved in ethanol, and the temperature is raised to 45°C to obtain iron stearate-ethanol solution, then boric acid-ethanol solution and stearin Pour ferric acid-ethanol solution into a sealed reaction kettle, raise the temperature to 100°C, react under stirring conditions for 1.5h, then lower the temperature and release the pressure, and filter the obtained slurry to obtain the ferroboron compound;

[0045] (2) adding lithium carbonate and water to the boron-iron compound obtained in step (1), through mixing and grinding, grinding to a slurry particle size of 250nm, and then spray drying to obtain a spray-dried material, which is calcined, The calcining temperature is 500°C, and the time is 7 hours to obtain the calcined material;

[0046] (3) The calcined material obtained in ste...

Embodiment 2

[0061] A preparation method of composite lithium iron borate, which is the following steps:

[0062] (1) Boric acid is dissolved in ethanol to obtain boric acid-ethanol solution, iron stearate is dissolved in ethanol, and the temperature is raised to 40°C to obtain iron stearate-ethanol solution, then boric acid-ethanol solution and stearin Pour the ferric acid-ethanol solution into a sealed reaction kettle, raise the temperature to 90°C, react for 1 hour under stirring conditions, then lower the temperature and release the pressure, and filter the obtained slurry to obtain the ferroboron compound;

[0063] (2) adding lithium carbonate and water to the boron-iron compound obtained in step (1), through mixing and grinding, grinding to a slurry particle size of 200nm, and then spray-drying to obtain a spray-dried material, which is calcined, The calcining temperature is 450°C and the time is 5h to obtain the calcined material;

[0064] (3) The calcined material obtained in step...

Embodiment 3

[0077] A preparation method of composite lithium iron borate, which is the following steps:

[0078] (1) Boric acid is dissolved in ethanol to obtain boric acid-ethanol solution, iron stearate is dissolved in ethanol, and the temperature is raised to 50°C to obtain iron stearate-ethanol solution, then boric acid-ethanol solution and stearin Pour the ferric acid-ethanol solution into a sealed reaction kettle, raise the temperature to 110°C, react for 2 hours under stirring conditions, then lower the temperature and release the pressure, and filter the obtained slurry to obtain the ferroboron compound;

[0079] (2) adding lithium carbonate and water to the boron-iron compound obtained in step (1), through mixing and grinding, grinding to a slurry particle size of 300nm, and then spray drying to obtain a spray-dried material, which is calcined, The calcining temperature is 550° C., and the time is 8 hours to obtain the calcined material;

[0080] (3) The calcined material obtain...

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Abstract

The invention discloses a preparation method of composite lithium iron borate. The preparation method comprises the steps: carrying out a reaction on a boric acid-ethanol solution with an iron stearate-ethanol solution at high temperature to obtain a ferroboron compound; adding lithium carbonate and water into the ferroboron compound, mixing, grinding and spray-drying to obtain a spray-dried material, and calcining the spray-dried material to obtain a calcined material; crushing the calcined material, adding a ferrous gluconate solution, lithium dihydrogen phosphate and ultrafine iron boride,mixing, grinding, spray-drying, calcining in a nitrogen atmosphere, carrying out jet milling, screening in a constant-temperature and constant-humidity room, carrying out vacuum packaging, and thus obtaining the product. The preparation method of composite lithium iron borate has good stability and good electrochemical performance, the 0.1 C discharge capacity of the finally prepared composite lithium iron borate is greater than or equal to 190 mAh / g, the stability is far higher than that of carbon-directly-coated lithium iron borate, the electrical performance is higher than that of lithium iron phosphate, and the composite lithium iron borate is an excellent lithium battery positive electrode material and is simple in preparation method and basically free of wastewater generation.

Description

technical field [0001] The invention relates to a preparation method of composite 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] The product obtained by the current conventional method has a large specific surface area, which is easy to absorb moisture an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45C01B35/12H01M4/36H01M4/58H01M10/052
CPCC01B25/45C01B35/128C01P2004/03C01P2004/62C01P2006/11C01P2006/12H01M4/366H01M4/5825H01M10/052H01M2004/028Y02E60/10
Inventor 蒋达金
Owner 蒋达金
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