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Method for preparing lithium iron phosphate-doped nano powder for lithium ion battery

A lithium-ion battery, lithium iron phosphate technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of powder agglomeration, high requirements for reaction atmosphere, poor reaction uniformity, etc. Uniform phase and small particle size

Inactive Publication Date: 2011-02-02
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the solid-phase method and the sol-gel method require high-temperature heat treatment for crystallization. On the one hand, there are high requirements on the reaction atmosphere, which is likely to cause poor reaction uniformity. On the other hand, high-temperature heat treatment inevitably causes powder agglomeration. Thereby affecting the application performance of the powder

Method used

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  • Method for preparing lithium iron phosphate-doped nano powder for lithium ion battery
  • Method for preparing lithium iron phosphate-doped nano powder for lithium ion battery
  • Method for preparing lithium iron phosphate-doped nano powder for lithium ion battery

Examples

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Effect test

Embodiment 1

[0021] 1) Synthesis of reaction precursors

[0022] Phosphoric acid, ferrous acetate and lithium hydroxide are formulated into a 0.4mol / L precursor solution according to the P:Fe:Li molar ratio of 1::1:1 (the solvent is water, and the following solvents all use water) ;

[0023] 2) Preparation of dopant source precursor solution

[0024] Prepare titanyl sulfate into a 0.5mol / L solution as the dopant source precursor;

[0025] 3) Mix the above doping source precursor solution and precursor solution according to the ratio of titanyl sulfate and ferrous ion molar ratio of 0.01:1, then put them in a hydrothermal reaction kettle, blow the inside of the kettle with high-purity nitrogen for 3 minutes, and then add 8MPa initial pressure, then react at 100°C for 20 hours, take it out after natural cooling, and then dry it after centrifugal washing to obtain a well-crystallized doped lithium iron phosphate nanopowder.

Embodiment 2

[0027] The first step is to synthesize the precursor solution: the phosphorus source compound (ammonium dihydrogen phosphate: phosphoric acid = 1: 1), ferrous chloride and lithium carbonate are formulated according to the ratio of P: Fe: Li molar ratio of 1: 1: 1 1.4mol / L precursor solution;

[0028] The second step is the preparation of the doping source precursor solution: nickel phosphate is prepared into a 1mol / L solution as the doping source precursor solution, and the doping source is nickel phosphate;

[0029] The third step is to mix the dopant source precursor solution with the precursor solution in a molar ratio of 0.1:1 and then place it in a hydrothermal reaction kettle. Blow the inside of the kettle with high-purity nitrogen for 3 minutes and then add an initial pressure of 4 MPa, and then After reacting at 180°C for 8 hours, take it out after natural cooling, then centrifuge, wash and dry to obtain a well-crystallized doped lithium iron phosphate nanopowder.

[...

Embodiment 3

[0032] The first step, synthetic precursor solution: phosphorus source compound (by diammonium hydrogen phosphate: phosphoric acid is mixed as 1: 1 in molar ratio): ferrous sulfate: lithium source compound (by lithium chloride and lithium acetate in molar ratio 1:1 mixing) according to the ratio of P:Fe:Li molar ratio of 1::1:1 to prepare a 2.4mol / L precursor solution (the solvent is water, and the following solvents all use water);

[0033] The second step is the preparation of the doping source precursor solution: the doping source is prepared into a 0.8mol / L solution, and the doping source is nickel phosphate,

[0034] Step 3: Mix the dopant source precursor solution with the precursor solution at a molar ratio of 0.08:1 and place it in a hydrothermal reaction kettle. Blow the inside of the kettle with high-purity nitrogen for 3 minutes and add an initial pressure of 2 MPa. After reacting at 220°C for 5 hours, take it out after natural cooling, then centrifuge, wash and dry...

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Abstract

The invention discloses a method for preparing lithium iron phosphate-doped nano powder for a lithium ion battery. The method comprises the following steps of: synthesizing precursor solution by using phosphorous source compounds, ferrous source compounds and lithium source compounds; preparing source-doped precursor liquid; mixing the source-doped precursor liquid and the precursor solution according to proportion; placing the mixture into a hydro-thermal reaction kettle, reacting at the temperature of between 100 and 220 DEG C under a nitrogen-containing and pressing environment; after the reaction, naturally cooling and taking the mixture out; and performing centrifugal washing on the mixture and drying the mixture to obtain the lithium iron phosphate-doped nano powder. In the method, the lithium iron phosphate-doped nano powder for the lithium ion battery is prepared by a hydrothermal method and by performing a chemical reaction in fluid such as high-temperature and high-pressure aqueous solution or water vapor and the like. Compared with a solid phase method and a sol-gel method, the method has the advantages of simple operation, uniform phase and small grain diameter.

Description

technical field [0001] The invention belongs to the field of new material technology and new energy technology, and relates to a nano-powder for lithium-ion battery technology, in particular to a preparation method for a lithium-ion battery-doped lithium iron phosphate nano-powder. Background technique [0002] As a new generation of chemical power sources, green and environmentally friendly lithium-ion secondary batteries are showing more and more development prospects, and their application fields are also expanding. At present, the cathode material of commercial lithium-ion batteries is mainly LiCoO 2 . Due to the extremely low content of Co in nature and its high price, its future development is restricted. Therefore, excellent electrical properties are sought. Inexpensive cathode materials are a very urgent task. Since LiFePO 4 With the advantages of low price, good safety performance and thermal stability, no pollution and high mass specific energy, it has become ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 刘文秀
Owner IRICO
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