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Synthesis method of high-purity fluorine-doped lithium iron phosphate anode material

A technology of electrode materials and mixtures, which is applied in the field of controllable synthesis of high-purity fluorine-doped lithium iron phosphate cathode materials, can solve the problems of low product purity and expensive raw materials, and achieve simple synthesis process, low price and high yield high effect

Inactive Publication Date: 2010-10-20
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a controllable synthesis method of a high-purity fluorine-doped lithium iron phosphate positive electrode material in order to solve the problems of expensive raw materials used in the traditional F doping modification method and the purity of the obtained product is not high.

Method used

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  • Synthesis method of high-purity fluorine-doped lithium iron phosphate anode material
  • Synthesis method of high-purity fluorine-doped lithium iron phosphate anode material
  • Synthesis method of high-purity fluorine-doped lithium iron phosphate anode material

Examples

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Effect test

Embodiment 1

[0024] LiFe(PO 4 ) 0.996 f 0.01 Preparation of / C material

[0025] Step 1: Put the analytically pure reagent LiOH·H 2 O, FeC 2 o 4 2H 2 O, NH 4 h 2 PO 4 and LiF, mixed according to the stoichiometric ratio of 1.01:1:0.996:0.01, adding 10% sucrose of the final product mass, using absolute ethanol as the medium, milling in a ball mill at a speed of 450r / min for 11h, and drying for 15h to obtain the mixture .

[0026] Step 2: Put the mixture prepared in Step 1 into the porcelain ark, and raise the temperature to 350°C at 10°C / min in a tube furnace under an argon atmosphere, keep it warm for 7 hours, and then raise it to 650°C at 10°C / min ℃, sintered for 15 hours, and the product was taken out when it was cooled to room temperature, and the final product was obtained.

Embodiment 2

[0028] LiFe(PO 4 ) 0.993 f 0.02 Preparation of / C material

[0029] Step 1: Put the analytically pure reagent LiOH·H 2 O, FeC 2 o 4 2H 2 O, NH 4 h 2 PO 4 and LiF, mixed according to the stoichiometric ratio of 1:1:0.993:0.02, adding 10% sucrose of the final product mass, using absolute ethanol as the medium, ball milling at a speed of 450r / min in a ball mill for 11h, and drying for 15h to obtain the mixture .

[0030] Step 2: Put the mixture prepared in Step 1 into the porcelain ark, and raise the temperature to 300°C at 10°C / min in a tube furnace under an argon atmosphere, keep it warm for 5 hours, and then raise it to 650°C at 10°C / min ℃, sintered for 10h, and the product was taken out when it cooled to room temperature, and the final product was obtained.

Embodiment 3

[0032] LiFe(PO 4 ) 0.99 f 0.03 Preparation of / C material

[0033] Step 1: Put the analytically pure reagent LiOH·H 2 O, FeC 2 o 4 2H 2 O, NH 4 h 2 PO 4 and LiF, mixed according to the stoichiometric ratio of 0.99:1:0.99:0.03, adding 10% sucrose of the final product mass, using absolute ethanol as the medium, milling in a ball mill at a speed of 450r / min for 11h, and drying for 15h to obtain the mixture .

[0034]Step 2: Put the mixture prepared in Step 1 into the porcelain ark, and raise the temperature to 350°C at 15°C / min in a tube furnace under an argon atmosphere, keep it warm for 6 hours, and then raise it to 650°C at 15°C / min ℃, sintered for 12 hours, and the product was taken out when it was cooled to room temperature, and the final product was obtained.

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Abstract

The invention relates to a synthesis method of high-purity fluorine-doped lithium iron phosphate anode material, which belongs to the field of the electro-chemistry energy storage material. The invention relates to an F-doped in-situ wrapped LiFePO4 material, i.e. LiFe(PO4)1-x / 3Fx / C material. Analytical reagent LiOH.H2O, FeC2O4.2H2O, NH4H2PO4 is mixed with fluoride, carbon source is added into the mixture, and the mixture is spherically ground and dried to obtain a precursor. The precursor which is obtained in the previous step is roasted in two steps, and the precursor is firstly pre-heated and then is further roasted to obtain the product. The method has the advantages of low cost of raw materials, simple synthesis process, easy realization, high purity of product, high yield and the like; and has high magnification discharging performance and low-temperature discharging performance, and greatly improves the magnification performance, platform voltage and low-temperature performance of the LiFePO4 battery.

Description

technical field [0001] The invention relates to a controllable synthesis method of a high-purity fluorine-doped lithium iron phosphate cathode material, belonging to the field of electrochemical energy storage materials. Background technique [0002] As a new generation of positive electrode active materials for lithium-ion batteries with the most potential for development and application, olivine-structured phosphates (such as LiFePO 4 ) has the advantages of low price, environmental friendliness, excellent cycle performance, and outstanding safety. However, the biggest obstacle limiting the application of this material is its electronic conductivity and Li + The chemical diffusion coefficients are all low, so that the capacity decays greatly when the large current is discharged. Therefore, how to improve the diffusion coefficient of lithium ions, ion conductivity and improve LiFePO 4 The high-current charge-discharge performance of the material is an urgent problem to b...

Claims

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Application Information

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IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 吴伯荣张存中张颖杨照军吴锋陈实杨春巍姚经文
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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