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Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material

A technology of lithium iron silicate and positive electrode materials, applied in the direction of electrode manufacturing, battery electrodes, electrical components, etc., can solve problems such as difficult industrial production, unsuitable for industrial production, complex operating conditions, etc., and achieve good electrochemical performance and easy industrialization The effect of simple production and process flow

Active Publication Date: 2013-12-25
NANJING GUOXUAN BATTERY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently Li 2 FeSiO 4 The preparation of materials mainly adopts high-temperature solid-phase synthesis method. The advantage of this method is that the process is simple and easy to realize industrialization. However, because the reactants are not easy to mix uniformly, the particle size of the product is large and the distribution is uneven, and the shape is irregular, so there are batches. lack of stability
Compared with the high-temperature solid-phase synthesis method, the hydrothermal method can directly synthesize Li 2 FeSiO 4 It is also easy to control the shape and particle size of the material, but the hydrothermal method requires high-temperature and high-pressure equipment, and industrial production is difficult
The sol-gel method can make the reaction materials mix at the molecular level, the particle size of the product is uniform, and the electrochemical performance of the product obtained is excellent, but its operating conditions are complicated and the yield is low, so it is not suitable for industrial production

Method used

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  • Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material
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  • Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Add silicon tetrachloride to absolute ethanol to form a solution with a concentration of 0.1mol / L, and calibrate its concentration for later use;

[0029] (2) Take out 20L of the above solution and place it in a reaction vessel, add water dropwise while stirring to promote its hydrolysis into a transparent sol;

[0030] (3) In the above sol, according to Li:Fe:Si=2:1:1 (molar ratio), add the aqueous solution made of lithium acetate and the aqueous solution made of ferrous acetate, and then add the solution made of sodium hydroxide. The aqueous solution forms a light green emulsion. At this time, the alkali concentration of the reaction system is controlled at 5mol / L, and the aging reaction is carried out in a hot water bath at 90°C and stirred for 8 hours;

[0031] (4) Washing the aged light green emulsion with an inorganic ceramic membrane to obtain a slurry liquid that removes impurity ions brought in by the raw material;

[0032] (5) Add the aqueous solution mad...

Embodiment 2

[0038] (1) Add silicon tetrachloride to absolute ethanol to form a solution with a concentration of 1.5mol / L, and calibrate its concentration for later use;

[0039] (2) Take out 20L of the above solution and place it in a reaction vessel, add water dropwise while stirring to promote its hydrolysis into a transparent sol;

[0040] (3) In the above sol, according to Li:Fe:Si=2:1:1 (molar ratio), add the aqueous solution made of lithium nitrate and the aqueous solution made of ferrous nitrate, and then add the solution made of potassium hydroxide. The aqueous solution forms a light green emulsion. At this time, the alkali concentration of the reaction system is controlled at 8mol / L, and the aging reaction is carried out in a hot water bath at 80°C and stirred for 6.5h;

[0041] (4) Washing the aged light green emulsion with an inorganic ceramic membrane to obtain a slurry liquid that removes impurity ions brought in by the raw material;

[0042] (5) Add the aqueous solution mad...

Embodiment 3

[0047] (1) Add silicon tetrachloride to absolute ethanol to form a solution with a concentration of 3mol / L, and calibrate its concentration for later use;

[0048] (2) Take out 20L of the above solution and place it in a reaction vessel, add water dropwise while stirring to promote its hydrolysis into a transparent sol;

[0049] (3) In the above sol, according to Li:Fe:Si=2:1:1 (molar ratio), add the aqueous solution made of lithium hydroxide and the aqueous solution made of ferrous chloride, and then add potassium hydroxide to make it The resulting aqueous solution generates a light green emulsion. At this time, the alkali concentration of the reaction system is controlled at 10mol / L, and the aging reaction is carried out in a 70°C hot water bath and stirred for 5h;

[0050] (4) Washing the aged light green emulsion with an inorganic ceramic membrane to obtain a slurry liquid that removes impurity ions brought in by the raw material;

[0051] (5) Add the aqueous solution mad...

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Abstract

The invention discloses a sol precipitation preparation method for a carbon-coated lithium iron silicate cathode material. The method comprises the following steps: adding silicon tetrachloride into absolute ethanol to form a solution; dropwise adding water while stirring for promoting the solution to be hydrolyzed into transparent sol; adding a water solution prepared from a lithium source, a water solution prepared from a divalent iron source and a water solution prepared from strong alkali respectively to generate a light green emulsion; ageing for 5-8 hours by stirring in a hot water bath of 70-90 DEG C; washing by an inorganic ceramic membrane to obtain a slurry solution without impurity ions; adding a water-soluble carbon source into the slurry solution, fully and uniformly mixing, and carrying out spray-drying to obtain carbon-containing Li2FeSiO4 precursor powder; putting the precursor powder into a tubular furnace; sintering for 7-15 hours at the temperature of 650-800 DEG C under the protection of inert gas to obtain a nanocarbon-coated Li2FeSiO4 material. The material prepared by the method is small in particle size, narrow in particle size distribution, low in raw material price, simple in process and easy for industrial production.

Description

[0001] technical field [0002] The invention relates to the technical field of battery material preparation, in particular to a sol precipitation liquid phase synthesis method, in particular to a sol precipitation preparation method of carbon-coated lithium iron silicate cathode material. Background technique [0003] Since Li / LiCoO 2 Since the industrialization of batteries, lithium-ion batteries have been widely used in mobile communications, notebook computers, portable electric tools, and electric The car's preferred power source. LiCoO 2 The discharge voltage is high, the cycle performance is good, and the synthesis conditions are simple, but cobalt resources are scarce, expensive, and harmful to the environment, and the charge state of LiCoO 2 Poor thermal stability, limited to LiCoO 2 Development of lithium-ion batteries for the positive electrode. [0004] In LiCoO 2 Among the alternative materials, Li 2 FeSiO 4 The material has the advantages of good therma...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/58H01M4/1397
CPCY02E60/10
Inventor 何学刚刘兴亮刘大军
Owner NANJING GUOXUAN BATTERY CO LTD
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