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Preparation method for nano-micro structured ferric phosphate

A technology of iron orthophosphate and phosphoric acid solution, applied in structural parts, chemical instruments and methods, nanotechnology, etc., can solve the problems of different sizes of iron phosphate particles, difficult to control the size and morphology effectively, and achieve uniform size. control, excellent electrochemical performance, and the effect of improving rate performance

Active Publication Date: 2017-06-20
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, this method first acidifies ferrous sulfate, and then adjusts the pH with ammonia water. During the whole process, the pH value gradually increases. Ferric phosphate is precipitated, while other parts of the solution are formed slowly. Therefore, as the reaction time progresses, the size of ferric phosphate particles varies, and its size and shape are difficult to be effectively controlled.

Method used

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  • Preparation method for nano-micro structured ferric phosphate
  • Preparation method for nano-micro structured ferric phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0056] (1) be that ferrous sulfate and phosphoric acid that mol ratio is 1:1 are dissolved in water, stir, make ferrous ion concentration and be the mixed solution of 4mol / L; Be that the phosphoric acid solution of 1.5 is transferred in the reactor by pH, Add the mixed solution of ferrous sulfate and phosphoric acid, 2mol / L hydrogen peroxide solution and 2mol / L ammonia water into the phosphoric acid solution at the same time, the molar ratio of the added ferrous ion and hydrogen peroxide is 2:1, and the pH is controlled The reaction was carried out at 1.5, and the reaction was carried out at 25°C for 12 hours. After the reaction was complete, the aging was continued for 24 hours;

[0057] (2) The product obtained in step (1) is filtered, washed, and dried to obtain FePO 4 Hydrate precursor;

[0058] (3) Put the precursor obtained in step (2) in a muffle furnace and heat-treat at 600°C for 4 hours to obtain FePO 4 Material.

[0059] FePO prepared in this embodiment 4 Materi...

Embodiment 2

[0061] (1) Dissolve ferrous oxalate and ammonium dihydrogen phosphate with a molar ratio of 2:1 in a solution of water and ethanol, wherein the ethanol content is 5%, stir evenly, and make a mixed ferrous ion concentration of 3mol / L solution; the phosphoric acid solution with a pH of 1.9 is transferred to the reactor, and the mixed solution of ferrous oxalate and ammonium dihydrogen phosphate, 2mol / L of sodium hypochlorite and 3mol / L of ammonia are added to the phosphoric acid solution at the same time, and the added ferrous ions The molar ratio with sodium hypochlorite is 2:3, and the pH is controlled at 1.9 for the reaction, and the reaction is carried out at 35° C. for 25 hours. After the reaction is complete, continue aging for 10 hours;

[0062] (2) The product obtained in step (1) is filtered, washed, and dried to obtain FePO 4 Hydrate precursor;

[0063] (3) Put the precursor obtained in step (2) in a muffle furnace and heat-treat it at 700°C for 2 hours to obtain FeP...

Embodiment 3

[0066] (1) Dissolve the combination of ferrous oxalate and ferrous sulfate and phosphoric acid in the solution of water and ethanol according to the molar ratio of 2:3, wherein the ethanol content is 10%, and stir evenly to make the ferrous ion concentration 2mol / L The mixed solution; the phosphoric acid solution with a pH of 2.5 is transferred to the reactor, and the mixed solution of ferrous oxalate, ferrous sulfate and phosphoric acid, 2mol / L hydrogen peroxide solution and 2.5mol / L potassium hydroxide solution are simultaneously Add it into the phosphoric acid solution, the molar ratio of the added ferrous ion and hydrogen peroxide is 1:1, control the pH at 2.5 for the reaction, the reaction is carried out at 50°C for 4 hours, after the reaction is complete, continue to age for 20 hours;

[0067] (2) The product obtained in step (1) is filtered, washed, and dried to obtain FePO 4 Hydrate precursor;

[0068] (3) Put the precursor obtained in step (2) in a muffle furnace and...

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Abstract

The invention relates to a preparation method for ferric phosphate. A ferric phosphate hydrate precursor is synthesized by adopting a coprecipitation method; and the precursor is subjected to aging, washing, drying and heat treatment to obtain the ferric phosphate. By improving the preparation condition of the ferric phosphate, effective control on granular dimensions and appearance of the ferric phosphate is realized, and the ferric phosphate material with uniform granules, regular appearance, narrow grain diameter distribution range, uniform and controllable dimensions and the nano-micro structure can be further obtained; and the obtained ferric phosphate material can be used for preparation of a positive electrode material lithium iron phosphate of a lithium ion battery. The preparation method provided by the invention has mild reaction conditions, simple and flexible operation and low cost; and meanwhile, the yield is improved, and batch production and wide application prospect of the material are achieved.

Description

technical field [0001] The invention relates to the field of battery material preparation, in particular to a method for preparing ferric orthophosphate with nano-microstructure. Background technique [0002] With the vigorous development of new energy vehicles, the lithium-ion battery industry has entered a stage of rapid development. The key materials that affect the performance of lithium-ion batteries mainly include positive electrode materials, negative electrode materials, and electrolytes. Among them, the positive electrode material is currently the main factor limiting battery performance, and it is also the main factor accounting for the high cost of lithium-ion batteries, which is close to 40%. [0003] In recent years, olivine-type cathode materials have been studied the most, among which LiFePO 4 attracted more attention. Compared with the traditional lithium ion secondary power cathode material lithium cobalt oxide (LiCoO 2 ) compared with lithium iron phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525C01B25/37B82Y30/00
CPCB82Y30/00C01B25/375C01P2004/03C01P2004/52C01P2004/61H01M4/5825H01M10/0525Y02E60/10
Inventor 谭强强夏青
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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