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Method for preparing carbon-coated spherical nano lithium iron phosphate by liquid phase method

A lithium iron phosphate, nanotechnology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of complex process and long precursor processing time, achieve uniform particle size, excellent high-current discharge performance, and improve tap density. Effect

Inactive Publication Date: 2012-07-18
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time to treat the precursor and the process is complicated. Since the precursor is not lithium iron phosphate forming an olivine structure, it still needs a long follow-up high temperature treatment.

Method used

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  • Method for preparing carbon-coated spherical nano lithium iron phosphate by liquid phase method
  • Method for preparing carbon-coated spherical nano lithium iron phosphate by liquid phase method
  • Method for preparing carbon-coated spherical nano lithium iron phosphate by liquid phase method

Examples

Experimental program
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Effect test

example 1

[0023] Prepare 1mol.L according to Fe:P molar ratio of 1:1 -1 100ml of mixed aqueous solution of ferrous sulfate and phosphoric acid, put the mixed solution in a 500ml reaction vessel with a reflux condenser device, add 100ml of dimethyl sulfoxide and 10ml of 2% polyacrylamide solution successively, slowly add 3mol .L -1 Lithium hydroxide solution until the pH of the reaction solution was 7, then heated to the boiling point of the solution (108°C) for 2 hours, the product was filtered, washed with deionized water and absolute ethanol, and dried in vacuum at 100°C for 10 hours to obtain pure phase nano-lithium iron phosphate powder. The obtained powder is mixed with 20% glucose and placed in a tube furnace, carbonized and spheroidized at 600° C. for 3 hours under the protection of nitrogen, and the product of the present invention is obtained after cooling. The obtained product has a spherical appearance and a particle size of 50-200 nm ( figure 1 ), detected by XRD powder di...

example 2

[0026] Prepare 1mol.L according to Fe:P molar ratio of 1:1 -1100ml of mixed aqueous solution of ferrous sulfate and phosphoric acid, put the mixed solution in a 500ml reaction vessel with a reflux condenser device, add 200ml of dimethyl sulfoxide and 1g of sodium dodecylbenzenesulfonate successively, and slowly add 2mol.L -1 Lithium hydroxide solution until the pH of the reaction solution is 7, then heated to the boiling point of the solution (115°C) and reacted for 1 hour, the product was filtered, washed with deionized water and absolute ethanol, and dried in vacuum at 100°C for 10 hours to obtain nano Lithium iron phosphate powder, mix the obtained nano-powder with 15% sucrose and place it in a tube furnace at 95N 2 and 5%H 2 Under the protection of mixed gas, crystallize at a high temperature of 600°C for 2 hours, cool and pulverize to obtain the product of the present invention. The shape of the obtained sample is spherical, and the particle size is 80-250nm. 1C and 1...

example 3

[0028] Prepare 1mol.L according to Fe:P molar ratio of 1:1 -1 100ml of mixed aqueous solution of ferrous chloride and phosphoric acid, put the mixed solution in a 500ml reaction vessel with a reflux condenser device, add 100ml of ethylene glycol and 0.5g of cetyltrimethylammonium bromide successively, stir slowly Slowly add 2mol.L -1 Lithium hydroxide solution until the pH of the reaction solution is 6.5, then heated to the boiling point of the solution (106°C) for 2 hours, the product was filtered, washed with deionized water and absolute ethanol, and dried in vacuum at 100°C for 10 hours to obtain nano Lithium iron phosphate powder. The resulting nanopowder was mixed with 10% glucose and placed in a tube furnace at 95N 2 and 5%H 2 Under the protection of mixed gas, carbonize and spheroidize at 550°C for 3 hours, cool and pulverize to obtain the product of the present invention. The shape of the obtained sample is spherical, the particle size is 50-200nm, and the sample i...

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Abstract

The invention discloses a method for preparing carbon-coated spherical nano lithium iron phosphate by a liquid phase method. According to the method, a lithium iron phosphate powder body with an olivine structure is quickly produced in a normal pressure liquid phase, the nano lithium iron phosphate powder obtained by the reaction is mixed with an organic carbon source such as glucose, the resultant product can be carbonized and spherized at high temperature within a very short time under the protection of inert atmosphere to obtain the carbon-coated spherical nano lithium iron phosphate with a small and uniform particle size, and the particle size range is 50nm to 300nm. The technical scheme of the invention is as follows: a certain-concentration mixed aqueous solution of ferrous salt and phosphoric acid is prepared with an equimolar ratio, and is placed in a reactor, a high-boiling-point polar organic solvent such as dimethyl sulfoxide and crystal growth inhibitor, such as polyacrylamide, of 0.5-3% are added, and the volume ratio of the aqueous solution to the high-boiling-point polar organic solvent is 0.5-2:1; under stirring, a lithium hydroxide solution with a certain concentration is added slowly until the pH value of a reaction solution is 6 to 7, and then the solution is heated to the boiling point, and reacts under reflux for 0.5 to 3h; the product is conventionally filtered, washed, and dried in a vacuum to obtain a nano-lithium iron phosphate powder body; and then the generated nano-lithium iron phosphate powder and the organic carbon source such as the glucose are mixed and placed in a high-temperature furnace in which inert gas is introduced to be used as protective gas, and under the condition that the temperature is controlled between 500 and 700 DEG C, the resultant product is crystallized and spheroidized for 1 to 5h, and is cooled and then pulverized to obtain the product provided by the invention. The product provided by the invention is used for a cathode material of lithium-ion batteries.

Description

technical field [0001] The invention belongs to a preparation method of a positive electrode material of a lithium ion battery, in particular to a method for directly preparing carbon-coated nanometer lithium iron phosphate powder under normal pressure liquid phase conditions. Background technique [0002] The theoretical capacity of lithium iron phosphate is 170mAh / g, and the discharge voltage is 3.4V. It has excellent safety performance and cycle performance, and the material has a wide range of raw materials, low price, and no pollution to the environment. It is considered to be a power lithium-ion battery with great potential. Materials have become a hot spot in research and development in recent years. However, lithium iron phosphate itself also has some defects. The first is that its special structure hinders the deintercalation rate of lithium ions; the second is that the electronic conductivity is poor, resulting in poor high-rate discharge performance; the third is ...

Claims

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Application Information

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IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 常照荣刘瑶李苞汤宏伟赵海丽黄静
Owner HENAN NORMAL UNIV
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