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A method for preparing lithium iron phosphate by inclusion process

A lithium iron phosphate and process technology, which is applied in the field of chemical synthesis materials, can solve the problems of poor electrical conductivity of materials and affect material properties, and achieve the effects of simple and easy method, complete and uniform coating, and stable performance.

Active Publication Date: 2016-08-10
南阳逢源新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the lithium iron phosphate molecule is so small, how to cover the nano-scale molecules evenly, instead of covering them very thickly, the conductive performance of the uncoated part of the material is still not good, which affects the overall performance of the material

Method used

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  • A method for preparing lithium iron phosphate by inclusion process
  • A method for preparing lithium iron phosphate by inclusion process
  • A method for preparing lithium iron phosphate by inclusion process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The invention provides a method for preparing lithium iron phosphate by clathrate technology, which is characterized in that it comprises the following steps:

[0019] ① Weigh the soluble phosphorus source compound, iron source compound, lithium source compound and clathrate at a molar ratio of 1:1:2 to 3.6:1, then supersaturated dissolve them in deionized water or distilled water to form phosphorus sources respectively Compound solution, iron source compound solution, lithium source compound solution, clathrate solution;

[0020] ② Add the phosphorus source compound solution into the autoclave, raise the temperature of the autoclave to 50-110°C, then slowly add the iron source compound solution into the autoclave, feed inert gas into the autoclave, and then slowly inject the Add the lithium source compound solution, and finally slowly add the clathrate solution into the autoclave, then seal the autoclave, set the temperature in the autoclave to rise to 120-260 °C at a ...

Embodiment 2

[0025] A method for preparing lithium iron phosphate by inclusion process is characterized in that it comprises the following steps:

[0026] ① First weigh the soluble phosphorus source compound, iron source compound and lithium source compound according to the molar ratio, and supersaturated dissolve the weighed soluble phosphorus source compound, iron source compound and lithium source compound in deionized water or distilled water to form Molecular-level phosphorus source compound precursor solution, iron source compound precursor solution, and lithium source compound precursor solution, and then use a hydrothermal method to make the phosphorus source compound precursor solution, iron source compound precursor solution, and lithium source compound precursor The precursor of lithium iron phosphate was synthesized in an autoclave using the bulk solution;

[0027] ②Separate the contents of the autoclave from solid to liquid, and the obtained solid is the lithium iron phosphate...

Embodiment 3

[0033] (1) Weigh and dissolve ferrous sulfate heptahydrate, phosphoric acid, lithium hydroxide monohydrate and β-cyclodextrin at a molar ratio of 1:1:3:1, and the total solid content is 10% of that of the solvent water. %.

[0034] (2) Add the phosphoric acid solution and the ferrous sulfate heptahydrate solution into the autoclave to mix them with strong high-speed stirring, then slowly add the lithium hydroxide solution into the autoclave, pass in an inert protective gas, and finally add β-cyclodextrin to seal The reaction kettle starts to heat up at a rate of about 3°C / min, rising to 220°C, keeping the temperature of the reaction system at 220°C, and controlling the system pressure at 1.6MPa. The constant temperature time is controlled at 8 hours.

[0035] (3) After the reaction, the solid and liquid are separated by centrifugation or suction filtration. The separated solid is washed to obtain a lithium iron phosphate clathrate crystal precursor.

[0036] (4) Add the lit...

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Abstract

The invention relates to a method for preparing lithium iron phosphate by a clathration technology. The method comprises the following steps of carrying out lithium iron phosphate crystal clathration by beta-cyclodextrin or hydroquinone as a clathrate and then carrying out carbonization annealing heat-treatment. The method has two good implementation methods and can realize clathration of lithium iron phosphate crystals in two stages. The method solves the problems of nonuniform and untight coating and realizes molecular grade clathration carbonization. The method effectively solves the problem of molecular agglomeration of lithium iron phosphate in synthesis and realizes refinement of secondary subgrain sizes. The lithium iron phosphate material obtained by the method has good nanometer particle size distribution and has an average particle size less than 1 micron. The lithium iron phosphate material has good conductive performances, realizes uniform and complete surface carbon coating, and has stable performances and gram volume of 163mAH. The method is simple and easy and is convenient for large-scale production.

Description

technical field [0001] The invention relates to the field of chemical synthesis materials, in particular to a method for preparing high-quality lithium iron phosphate crystals for lithium ion secondary battery anode materials by inclusion process. Background technique [0002] Since Japan's NTT first revealed AyMPO in 1996 4 (A is an alkali metal, M is a combination of CoFe: LiFeCOPO 4 ) Lithium battery cathode material with olivine structure, in 1997, John.B.Goodenough and other research groups at Texas State University reported LiFePO 4 The olivine structure (LiMPO 4 ), Europeans also discovered LiFePO with natural olivine structure 4 . LiFePO 4 It has also been found to have superior performance that cannot be compared with commercialized secondary battery materials such as lithium cobalt oxide, lithium nickel oxide, and ternary materials. The material has a series of advantages such as wide source of raw materials, low price, no memory effect, long cycle life, good...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58C01B25/45
CPCC01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 孙青林汪浩魏宏政
Owner 南阳逢源新能源科技有限公司