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Preparation method of lithium ion battery anode material lithium fluoborate

A lithium ferrous borate and lithium-ion battery technology, which is applied in battery electrodes, borates, circuits, etc., can solve the problems that are not conducive to energy conservation and environmental protection, high sintering temperature, poor controllability, etc., and achieve regular shape and high sintering temperature. low cost, easy operation

Active Publication Date: 2014-02-05
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is complex in process, poor in controllability, high in sintering temperature, and high in energy consumption, which is not conducive to energy saving and environmental protection

Method used

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  • Preparation method of lithium ion battery anode material lithium fluoborate
  • Preparation method of lithium ion battery anode material lithium fluoborate
  • Preparation method of lithium ion battery anode material lithium fluoborate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 0.1mol lithium hydroxide, 0.1mol ferric nitrate, 0.025mol ammonium tetraborate and 0.013mol citric acid in 200mL water, stir in a constant temperature water bath at 80°C for 1.5h to obtain a sol, and then stand at this temperature for 0.5h. Make it form a gel, then add water to the original scale of the container to replenish the evaporated water, stir evenly and then spray dry to obtain the precursor. The inlet temperature of the spray drying process is 220°C, the outlet temperature is 130°C, and the feed rate is 1000mL h -1 ; Then place the precursor in a magnetic boat for compaction, put it in a tubular sintering furnace and sinter at 300°C for 2h under the protection of nitrogen, then continue to heat up to 500°C for 10h, and cool naturally to room temperature to obtain LiFeBO 3 .

[0026] The XRD diffraction pattern of the sample obtained in this embodiment is shown in figure 1 , the SEM images of the obtained samples are shown in figure 2 . The obta...

Embodiment 2

[0028] Dissolve 0.021mol of lithium acetate, 0.02mol of iron triacetylacetonate, 0.02mol of boric acid, and 0.0075mol of tartaric acid in 200mL of water, stir in a constant temperature water bath at 70°C for 2.5h to obtain a sol, and then stand at this temperature for 0.4h to make it Form a gel, then add water to the original scale of the container to replenish the evaporated water, stir well and then spray dry to obtain the precursor. The inlet temperature of the spray drying process is 220°C, the outlet temperature is 130°C, and the feed rate is 1000mL·h -1 ; Then put the precursor in a magnetic boat for compaction, put it in a tubular sintering furnace and sinter at 300°C for 2.5h under the protection of argon, then continue to heat up to 450°C for 12h, and cool naturally to room temperature to obtain LiFeBO 3 .

[0029] The obtained product is used as the positive electrode material, and the metal lithium sheet is used as the negative electrode material, and assembled into...

Embodiment 3

[0031] Dissolve 0.0612mol of lithium nitrate, 0.06mol of ferrous oxalate, 0.03mol of diboron trioxide, and 0.015mol of oxalic acid in 200mL of water, stir in a constant temperature water bath at 80°C for 2h to obtain a sol, and then stand at this temperature for 0.5h , to make it form a gel, then add water to the original scale of the container to replenish the evaporated water, stir evenly and then spray dry to obtain the precursor, the inlet temperature of the spray drying process is 220°C, the outlet temperature is 130°C, and the feed rate is 1000mL·h -1 ; Then put the precursor in a magnetic boat for compaction, put it in a tubular sintering furnace and sinter at 350°C for 2h under the protection of argon, then continue to heat up to 550°C for 5h, and cool naturally to room temperature to obtain LiFeBO 3 .

[0032] The obtained product is used as the positive electrode material, and the metal lithium sheet is used as the negative electrode material, and assembled into a C...

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Abstract

The invention discloses a preparation method of a lithium ion battery anode material lithium fluoborate. The preparation method comprises the following steps: (1), mixing a lithium source, an iron source, a boron source and a chelating agent according to the condition that the molar ratio of Li, Fe, B and C is (1-1.05):1:1:(0.5-1.5), adding the mixture into water for dissolving, and controlling the concentration of metal ions at 0.1-0.8mol / L<-1> to obtain liquor; (2), stirring in constant-temperature water bath to form sol; (3), stewing at the constant temperature to form gel; (4), adding water into the gel, and stirring; (5), spraying and drying to obtain a precursor; (6), sintering the precursor for 1.5 hours-2.5 hours at 250 DEG C-350 DEG C in a non-oxidizing atmosphere, then, heating up to 450 DEG C-550 DEG C, sintering for 5 hours-12 hours, and naturally cooling to the room temperature, thereby obtaining LiFeBO3. According to the preparation method disclosed by the invention, material resource is extensive, the operation is simple, convenient and easy to implement, the controllability is strong, the sintering temperature is low and the production cost is low.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material of a lithium ion battery, in particular to a preparation method of lithium ferrous borate, a positive electrode material of a lithium ion battery. Background technique [0002] LiFeBO 3 It is a new type of cathode material for lithium-ion batteries. It has a high specific capacity (~220mAh g -1 ), good electrical conductivity (conductivity ~ 3.9×10 -7 S cm -1 ), a very small volume change rate (~2%), at the same time, borate (B0 3 ) 3- Has a small molar mass (58.8), much smaller than the same kind of phosphate (P0 4 ) 3- Polyanion (95), and its structure can provide lithium ion conduction and electron conduction at the same time, so it has become a hot spot of recent research. At the same time, the content of iron in the earth's crust is very high, ranking fourth after oxygen, silicon, and aluminum, with an abundance of 4.75%. my country is also a country with large ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12H01M4/58H01M4/136
CPCY02E60/122Y02E60/10
Inventor 郑俊超张宝明磊张佳峰韩亚东沈超王健龙
Owner CENT SOUTH UNIV
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