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Preparation method of lithium iron phosphate oxide of cathode material of lithium ion battery

A technology for lithium-ion batteries and cathode materials, applied in phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., to achieve the effects of simple operation process, easy control, and simple equipment

Inactive Publication Date: 2010-02-03
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of lithium iron phosphate oxide of cathode material of lithium ion battery
  • Preparation method of lithium iron phosphate oxide of cathode material of lithium ion battery
  • Preparation method of lithium iron phosphate oxide of cathode material of lithium ion battery

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Embodiment 1

[0017] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 0.2L deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution At the same time, it was added to the reactor at a speed of 800mL / h, and the stirrer was turned on for strong stirring. The reaction temperature was controlled at 80°C, and the reaction was carried out for 0.5h at a stirring speed of 800r / min to obtain a suspension of gray ferrous phosphate Turbid liquid; take 11.4mL of hydrogen peroxide and add it to the above suspension, a large amount of white precipitates will appear immediately, continue to react for 0.5h, and after aging for 6h, filter and wash repeatedly to obtain precipitate iron phosphate; Dry in a drying oven at 120°C for 12 hours to obtain 35.8g of dried FePO 4 2H 2 O powder;

[0018] (2) Preparation of lithium iron phosphorus oxide: take the dried FePO 4 2H 2 18.7g o...

Embodiment 2

[0021] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 2L of deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution simultaneously Add it into the reactor at a speed of 400mL / h, and turn on the stirrer for strong stirring, control the reaction temperature at 70°C, and under the condition of stirring speed of 1200r / min, the reaction time is 2h, and the suspension of gray ferrous phosphate is obtained. Turbid liquid: Take 15.6 mL of hydrogen peroxide and add it to the above suspension, a large amount of white precipitates will appear immediately, continue to react for 2 hours, and after aging for 8 hours, filter and wash repeatedly to obtain precipitated ferric phosphate. According to the prior art, dry at 60-120°C for 5-20h in a blast oven; obtain dry FePO 4 2H 2 O powder 35.5g;

[0022] (2) Preparation of lithium iron phosphorus oxide: dry FeP...

Embodiment 3

[0025] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 0.1L deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution At the same time, it was added to the reactor at a speed of 1200mL / h, and the stirrer was turned on for stirring. The reaction temperature was controlled at 90°C. Under the condition of stirring speed of 400r / min, the reaction time was 0.3h, and a suspension of gray ferrous phosphate was obtained. Turbid solution: Take 11.4mL of hydrogen peroxide and add it to the above suspension. Immediately, a large amount of white precipitates are formed. Continue to react for 0.3h, and after aging for 4h, filter and wash repeatedly to obtain precipitated ferric phosphate. After separation, dry at 120°C for 12 hours in a blast drying oven to obtain 34.6 g of dried FePO 4 2H 2 O powder;

[0026] (2) Preparation of lithium iron phosphorus oxide:...

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Abstract

The invention discloses a preparation method of lithium iron phosphate oxide of cathode material of a lithium ion battery, which comprises the following steps: adding ferrous ion aqueous solution withthe concentration of 0.05-2mol / L and ammonium dihydrogen phosphate solution into a reactor according to the ratio of 1: 1; reacting for 0.2-2h under the conditions that the reaction temperature is 50-90 DEG C and the stirring speed is 400-1200rpm; adding excessive hydrogen peroxide and reacting for 0.2-2h, and ageing, filtering, washing and drying to obtain precursor iron phosphate powder; mixingthe iron phosphate powder, lithium ions in a lithium source and carbon atoms in a carbon source according to the mol ratio of 2: 2: 0.1-0.6 by taking absolute ethanol as a medium, and then putting into a planetary ball mill for grinding to obtain precursor solution of the lithium iron phosphate oxide; and then roasting to obtain the lithium iron phosphate oxide with the particle diameter of 0.5-5Mum. The product prepared by the method has even and fine particle diameter distribution, high reaction activity, simple and convenient operation process, simple device and easy control, and effectively improves the electrochemical property and reduces the cost.

Description

technical field [0001] The invention relates to a preparation method of iron phosphate, a lithium iron phosphate precursor, which is a cathode material of a lithium ion battery. Background technique [0002] Currently preparing LiFePO 4 The methods can be roughly divided into solid phase synthesis and soft chemical synthesis, in addition to pulse laser precipitation, spray pyrolysis and so on. Materials synthesized by different synthesis methods or under different synthesis conditions will have different shapes and properties. The synthesis temperature of the solid phase method is high, the energy consumption is large, the phase is not uniform, the crystal size is large, the particle size distribution range is wide, and the calcination time is long; the cost of the sol-gel method is high, the operation process is complicated, and it is difficult to industrialize; microwave The hydrothermal method has high requirements on equipment, large investment, difficult process contr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45
Inventor 彭春丽张佳峰沈超
Owner CENT SOUTH UNIV
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