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Lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and preparation method thereof

A technology of lithium iron phosphate and positive electrode materials, applied in the direction of positive electrodes, nanotechnology for materials and surface science, battery electrodes, etc., can solve the problems affecting the electrochemical performance and cycle performance of batteries, small tap density volumetric energy density, Problems such as low ion diffusion coefficient, achieve excellent charge-discharge cycle performance, improve electronic conductivity, and avoid side reactions

Active Publication Date: 2019-07-16
湖北锂诺新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, LiFePO 4 There are some defects: (1) The lower electronic conductivity leads to the FePO in the outer layer during the delithiation process 4 It will hinder the migration of particles, which is not conducive to the internal LiFePO 4 (2) The ion diffusion coefficient is low; (3) The smaller tap density results in lower volumetric energy density

Method used

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  • Lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and preparation method thereof
  • Lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and preparation method thereof
  • Lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and preparation method thereof

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Effect test

Embodiment 1

[0014] Reagent: NH 4 h 2 PO 4 , Fe(NO 3 ) 3 9H 2 O, Li 2 CO 3 , Al(NO 3 ) 3 9H 2 O, LiNO 3 , NH 4 F, glucose, deionized water and ethanol.

[0015] Preparation of lithium iron phosphate powder: 1.15g NH 4 h 2 PO 4 , 4.04g Fe(NO 3 ) 3 9H 2 O was dissolved in 60mL of deionized water, added 2g of glucose, and stirred for 30min. The reaction occurred, reacted at 140°C for 6h, cooled naturally to room temperature, and washed with water and ethanol three times. The samples were dried in an oven at 60 °C for 12 h, and then calcined at 500 °C for 10 h in a tube furnace under the protection of nitrogen. The calcined sample was mixed with 0.74g Li 2 CO 3 Perform ball milling and mixing for 2 hours, then calcinate at 700°C for 10 hours in a nitrogen atmosphere, grind after cooling, and sieve to remove iron to obtain LiFePO 4 sample.

[0016] Co-doped LiFePO with Li, Al and F 4 Preparation of: 0.0683gAl(NO 3 ) 3 9H 2 O, 0.0126 g LiNO 3 and 0.0283gNH 4 Dissolve...

Embodiment 2

[0018] Preparation of lithium iron phosphate powder: 1.15gNH 4 h 2 PO 4 , 3.23gFe(NO 3 ) 3 9H 2 O was dissolved in 60ml deionized water, added 2.18 glucose, and stirred for 30min. The reaction occurred, reacted at 150°C for 8h, cooled naturally to room temperature, and washed with water and ethanol three times. The samples were dried in an oven at 80 °C for 14 h, and then calcined at 500 °C for 10 h in a tube furnace under the protection of nitrogen. The calcined sample was mixed with 0.81gLi 2 CO 3 Perform ball milling and mixing for 2 hours, then calcinate at 700°C for 10 hours in a nitrogen atmosphere, grind after cooling, and sieve to remove iron to obtain LiFePO 4 sample.

[0019] Co-doped LiFePO with Li, Al and F 4 Preparation of: 0.0750g Al(NO 3 ) 3 9H 2 O, 0.0138g LiNO 3 and 0.0296g NH 4 F was dissolved in deionized water and stirred for 1 h. Then add 1.14g LiFePO 4 The powder was stirred for 1 h. A reaction occurred and was kept at 160°C for 5h. Coo...

Embodiment 3

[0021] Preparation of lithium iron phosphate powder 1.15g NH 4 h 2 PO 4 , 4.84g Fe(NO 3 ) 3 9H 2 O was dissolved in 60 mL of deionized water, 1.82 g of glucose was added, and stirred for 30 min. The reaction occurred, reacted at 130°C for 8h, cooled naturally to room temperature, and washed with water and ethanol three times. The samples were dried in an oven at 70 °C for 13 h, and then calcined at 530 °C for 10 h in a tube furnace under the protection of argon. The calcined sample was mixed with 0.81g Li 2 CO 3 Perform ball milling and mixing for 2 hours, then calcinate at 700°C for 10 hours in a nitrogen atmosphere, grind after cooling, and sieve to remove iron to obtain LiFePO 4 sample.

[0022] Co-doped LiFePO with Li, Al and F 4 Preparation of: 0.0563g Al(NO 3 ) 3 9H 2 O, 0.0124 g LiNO 3 and 0.025g NH 4 Dissolve F in 30 mL deionized water and stir for 1 h. Then add 0.85g LiFePO 4The powder was stirred for 1 h. The mixture was transferred to a 50mL reacto...

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Abstract

The invention relates to a lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and a preparation method thereof; the preparation method comprises the following steps of enabling Al(NO3)3.9H2O, LiNO3 and NH4F to be dissolved in deionized water separately and performing uniform mixing; next, adding LiFePO4 powder to be reacted, wherein the molar ratio of Al(NO3)3.9H2O to LiNO3 to NH4F to LiFePO4 is 1 to (0.8-1.2) to (4-4.5) to (30-36), the reaction temperature is 150-160 DEG C, and the reaction time is 5-8h; carrying out washing and drying, wherein the drying temperature is 80-90 DEG C, and the drying time is 12-14h; and next, carrying out calcining, wherein the calcining temperature is 500-550 DEG C and the calcining time is 6-8h, to obtain the lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material. The conductivity of the prepared lithium iron phosphate positive electrode material is improved and the material isapplied to a battery, so that the electrochemical performance and the cycling performance of the battery are improved.

Description

technical field [0001] The invention relates to a lithium ion battery positive electrode material, in particular to a lithium, aluminum and fluorine co-doped lithium iron phosphate positive electrode material and a preparation method. Background technique [0002] Over the past few decades, the planet has been warmed by the greenhouse effect and limited fossil fuels. Therefore, scientists are actively developing new energy sources to replace them. Lithium-ion battery technology is very mature and commercialized. Olivine lithium iron phosphate (LiFePO 4 ) positive electrode material was first reported by the American Goodenough research group in 1997. with LiCoO 2 , LiNiO 2 and LiMnO 2 Compare, LiFePO 4 It has the advantages of higher theoretical discharge specific capacity (170mAh / g), discharge voltage platform of 3.4V, high energy density, good cycle performance, good safety, environmental friendliness and low cost. Therefore, LiFePO 4 The positive electrode materi...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62H01M10/0525B82Y30/00
CPCH01M4/5825H01M4/624H01M10/0525B82Y30/00H01M2004/021H01M2004/028Y02E60/10
Inventor 杨志远王聪蔡浩张天赐
Owner 湖北锂诺新能源科技有限公司
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