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Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material

A technology of micro-nano structure and iron phosphate salt, applied in structural parts, chemical instruments and methods, nanotechnology for materials and surface science, etc., can solve problems such as difficult to achieve high tap density, high rate and high capacity, and achieve Controllable structure and shape, excellent performance and high tap density

Active Publication Date: 2012-07-18
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods can improve some properties of lithium iron phosphate materials to a certain extent, it is still difficult to achieve a uniform combination of high tap density, high rate and high capacity.

Method used

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  • Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material
  • Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material
  • Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of micro-nano structure basic ammonium iron phosphate and iron phosphate

[0035] Use ferrous sulfate as the iron source, configure 1mol / L ferrous sulfate aqueous solution, weigh ammonium dihydrogen phosphate into the aqueous solution according to the stoichiometric ratio, use sulfuric acid to adjust the pH of the obtained solution to 2, and keep the temperature at 20°C. Reacting for 0.5 hours under the condition of stirring rate of 300rpm;

[0036] Control the stirring rate to 300rpm, measure the stoichiometric ratio of hydrogen peroxide, and add it dropwise to the mixed solution of ferrous sulfate and ammonium dihydrogen phosphate, and use ammonia water to adjust the system to PH = 2. After the addition, raise the temperature to 80°C to continue After reacting for 8 hours, it was centrifuged and washed until no sulfate group was detected with 30% barium chloride solution; the washed product was dried at 120°C for 4 hours to obtain a micronano-structure...

Embodiment 2

[0043] Prepare a 0.1mol / L ferrous nitrate solution, weigh diammonium hydrogen phosphate and add it to the aqueous solution according to the ferrous ion concentration and phosphate ion concentration of 0.8:1, use sulfuric acid to adjust the pH of the resulting solution to 3, and keep the temperature at 50 °C, reacted for 0.5 hours at a stirring rate of 500rpm; measure hydrogen peroxide with a stoichiometric excess of 10%, add it dropwise to the mixed solution of ferrous nitrate and diammonium hydrogen phosphate, and use ammonia water to adjust the system to PH=3, After the dropwise addition, keep the temperature at 50°C and continue the reaction for 14 hours. After centrifugation and washing, dry at 140°C for 2 hours to obtain a micro-nano structure basic ferric ammonium phosphate containing 1 crystalline water. The primary particle size is 30-50nm, the secondary particle size is about 3 microns. The obtained basic ammonium iron phosphate is heat-treated at 400° C. for 10 hours...

Embodiment 3

[0045] Prepare a mixed solution of 0.5mol / L ferrous chloride and ferrous acetate, the mass ratio of the two is 1:1, and add diammonium hydrogen phosphate to the aqueous solution according to the ferrous ion concentration and phosphate ion concentration of 1.2:1 , use ammonia water to adjust the pH of the resulting solution to 5, and keep the temperature at 80°C, and react for 1 hour at a stirring rate of 800rpm; measure hydrogen peroxide with a stoichiometric excess of 50%, and add it dropwise to ferrous chloride, acetic acid In the mixed solution of ferrous iron and diammonium hydrogen phosphate, use ammonia water to adjust the system pH=5 at the same time, keep the temperature at 80°C to continue the reaction for 4 hours after the dropwise addition, and dry at 100°C for 6 hours after centrifugation and washing to obtain The micro-nano structure basic ammonium ferric phosphate containing 2 crystal waters has a primary particle size of 20-30nm and a secondary particle size of a...

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Abstract

The invention relates to ferric phosphate having a micro-nano structure and a preparation method thereof as well as a lithium iron phosphate material. At least one dimension of a primary particle size of the ferric phosphate having the micro-nano structure in a three-dimensional space stays within a nanosecond range, an average size of the primary particles is 1nm to 100nm, and the size of a secondary particle consisting of the primary particles ranges between 0.5 to 10 micrometers. The preparation process is that: a phosphorus source is added into ferrous salt aqueous solution, oxidant is added under a blending condition, aqueous ammonia is used for controlling the systematic pH value to be 1 to 5, and a micro-nano structural particle with given grain fineness distribution is formed after being gathered and after the reaction for 2 to 72 hours under the temperature of 20 to 90 DEG C, and the micro-nano structure particles are washed, dried and roasted to obtain the ferric phosphate having the micro-nano structure. The preparation method has characteristics of simple process flow, good and stable product quality, low cost and the like. The lithium iron phosphate positive material which is prepared by utilizing the ferric phosphate having the micro-nano structure has excellent performance and has characteristics of high vibration density, good specific capacity, good circulation performance and the like.

Description

technical field [0001] The invention belongs to the technical field of energy storage materials, and specifically relates to a class of iron phosphate salts with a micro-nano structure and a preparation method thereof, and a lithium iron phosphate positive electrode material prepared based on the micro-nano structure iron phosphate salts, in particular to a lithium iron phosphate cathode material for the synthesis of iron phosphate Basic iron ammonium phosphate and iron phosphate with micro-nano structure of lithium and preparation method thereof. Background technique [0002] With the gradual depletion of fossil energy, new energy technology has attracted worldwide attention. Lithium-ion battery is a new generation of green high-energy battery with high energy density, large output power, high average output voltage, small self-discharge, no memory effect, fast charge and discharge, excellent cycle performance, and no environmental pollution. The preferred object of rechar...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B25/45H01M4/58H01M4/1397B82Y40/00B82Y30/00
CPCY02E60/122Y02E60/10
Inventor 刘兆平姚霞银袁国霞唐长林王军
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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