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Battery grade sheet hydrated iron phosphate and preparation method thereof

A technology of hydrated ferric phosphate and hydrated phosphoric acid, which is applied in battery electrodes, circuits, electrical components, etc., can solve the problems of low rate performance and poor low temperature performance of lithium iron phosphate materials, and is suitable for large-scale mass production and low cost , The effect of reducing product cost

Inactive Publication Date: 2013-04-03
PULEAD TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The first object of the present invention is to provide a lithium ion battery cathode material precursor, using a hydrated ferric phosphate with a growth advantage as the lithium ion battery cathode material precursor, to overcome the existing lithium ion cathode material precursor phosphoric acid The rate performance of lithium iron phosphate material prepared by iron material is not high, and the technical defects of existing lithium iron phosphate material are poor low temperature performance

Method used

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  • Battery grade sheet hydrated iron phosphate and preparation method thereof
  • Battery grade sheet hydrated iron phosphate and preparation method thereof
  • Battery grade sheet hydrated iron phosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 2g of cetyltrimethylammonium bromide, 13.90g of ferrous sulfate heptahydrate and 23.06g of concentrated phosphoric acid into 300ml of deionized water at room temperature, that is, the addition of surfactant is about 6.7g / L, iron The element concentration is 0.17mol / L, and the molar ratio of iron and phosphorus is 1:4.1. Then ultrasonically stir until completely dissolved. Then add 3.2g concentration of 28% hydrogen peroxide dropwise to the system. After the dropwise addition, continue to stir for 2 hours, and the pH value of the system is 1.2; The reaction system was filtered to obtain 289g of the filtrate, and the product was washed repeatedly with ethanol ultrasonics to obtain a powdery white precipitate; the powdery white precipitate was dried at 60°C for 8 hours to obtain 8.41g of the hydrated ferric phosphate of the present invention, with a yield of 90% .

[0034] Scanning and transmission electron microscope observations are carried out to obtaining hydra...

Embodiment 2

[0036]Weigh 3g of cetyltrimethylammonium bromide, 5.46g of pure iron powder, 1.7g of ammonium dihydrogen phosphate and 31.2g of concentrated phosphoric acid into 300ml of deionized water at room temperature, that is, the amount of surfactant added is about 10g / L, the concentration of iron element is 0.32mol / L, and the molar ratio of iron element and phosphorus element is 1:5.0. Then ultrasonically stir until completely dissolved. Then add 3.3g of hydrogen peroxide with a concentration of 29% dropwise into the system. After the dropwise addition, continue to stir for 1 hour, and the pH value of the system is 1.8; then heat up to 80°C, and continue the reaction for 12 hours under stirring. The reaction system was filtered to obtain 291 g of filtrate, and the product was washed repeatedly with ethanol ultrasonics to obtain a powdery white precipitate; the powdery white precipitate was dried at 65° C. for 7 hours to obtain 8.27 g of the hydrated ferric phosphate of the present in...

Embodiment 3

[0038] Take by weighing 0.5g cetyltrimethylammonium bromide, 8.99g ferrous oxalate dihydrate, 5.65g concentrated phosphoric acid and 9g deionized water at room temperature and add them to the 291g filtrate in Example 2, namely the added surface active The amount of the agent is about 1.7g / L, the concentration of iron element is 0.27mol / L, and the molar ratio of iron element and phosphorus element is 1:1.01. Then ultrasonically stir until completely dissolved. Then add 3.1 g of hydrogen peroxide with a concentration of 30% dropwise to the system. After the dropwise addition, continue to stir for 1.5 hours, and the pH of the system is 1.75; then heat up to 90° C., and continue the reaction for 6 hours under stirring. The reaction system was filtered to obtain 285 g of the filtrate, and the product was washed repeatedly with ethanol ultrasonics to obtain a light pink precipitate; the light pink precipitate was dried at 70°C for 5 hours to obtain 8.67 g of the hydrated ferric phos...

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Abstract

The invention relates to a lithium ion battery anode material precursor and a preparation method thereof. The precursor is sheet hydrated iron phosphate, and the preparation method comprises the following steps of: dissolving a surface active agent, an iron source compound and a phosphorus source compound in water to form a uniform and stable solution A, wherein the added quantity of the surface active agent is 2 to 10 g / L, the concentration of iron is 0.08 to 0.32 mol / L, the mole ratio of the iron to phosphorus is 1:X, and X is more than or equal to 3.0 and less than or equal to 5.0; adding oxydol into the solution A, and stirring to obtain a solution B; performing high-temperature reaction on the solution B to obtain a solution C; and filtering the solution C to obtain the hydrated iron phosphate. By the method, the sheet hydrated iron phosphate with a controllable shape can be prepared, thus the electrochemical performance of a lithium ion battery anode material namely lithium iron phosphate is improved; and the filtrate obtained in the preparation process can be recycled to improve the utilization ratio of raw materials.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials for lithium ion batteries, and in particular relates to a hydrated lithium iron phosphate precursor of a sheet-shaped lithium ion battery positive electrode material and a preparation method thereof. Background technique [0002] Since 1997, it was first reported by Goodenough (Padhi AK, Nanjundaswamy KS and Goodenough JB, J. Electrochem. Soc. 1997, 144:1188-1194) that lithium ions in lithium iron phosphate with olivine structure can be intercalated / extracted and used as lithium Since the positive electrode material of ion battery, based on the olivine structure (LiMPO 4 , M=Fe, Mn, Ni, Co, etc.) lithium-ion battery cathode materials, especially LiFePO 4 and its precursors have flourished. [0003] According to the current technology, the precursors of lithium iron phosphate mainly include iron-containing oxalate (patent application number: 200710034940.2), iron-containing o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 范永新张卫东周恒辉
Owner PULEAD TECH IND
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