Nano solid-core iron phosphate-carbon source-graphene composite material and preparation method thereof

A technology of solid iron phosphate and composite materials, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem that sulfate radicals damage the cycle performance of lithium iron phosphate, iron phosphate cannot reach the nanometer level, Increase the ferrous iron oxidation process and other issues to achieve the effect of facilitating large-scale industrialization, improving electronic conductivity, and shortening the synthesis process

Active Publication Date: 2014-11-26
吴位跃
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the electrochemical performance of lithium iron phosphate can be greatly improved, the raw material ferrous ammonium sulfate hexahydrate uses ferrous iron, which needs to increase the oxidation process of ferrous iron to ferric iron in iron phosphate, and the production cost is greatly increased. , and the sulfate used in ammonium ferrous sulfate hexahydrate is difficult to remove in the subsequent washing process, and the sulfate has a serious damage to the cycle performance of lithium iron phosphate
In addition, the surface of iron phosphate grown on graphene is not limited by cladding, and iron phosphate crystals are easily overgrown, resulting in the failure of iron phosphate to reach the nanoscale
Another major problem is that the ferric phosphate prepared by the inventive method is a hollow structure, which can cause the tap density of ferric phosphate to be greatly reduced, and the generation of lithium iron phosphate with ferric phosphate as a skeleton is also a hollow structure, and its tap density is greatly reduced. Reduced, resulting in low volume specific capacity, and the actual application value is greatly reduced

Method used

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  • Nano solid-core iron phosphate-carbon source-graphene composite material and preparation method thereof
  • Nano solid-core iron phosphate-carbon source-graphene composite material and preparation method thereof
  • Nano solid-core iron phosphate-carbon source-graphene composite material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Graphene oxide was ultrasonically dispersed with deionized water for 60 min to obtain a 1.5 mg / mL suspension. In 100mL deionized water, add 0.1mol Fe(NO 3 ) 3 , 0.1mol (NH 4 ) 2 HPO 4 , 5 g of PVA and 1 mL of graphene oxide suspension. The mixture was sonicated in a sonicator for 8 minutes and then placed in a reaction kettle. The constant stirring speed in the reactor was 50 rad / min. Concentrated ammonia solution was added dropwise to the solution, and the pH value of the mixed solution was adjusted to 3. The reaction temperature was kept at 60° C., and the reaction was carried out for 36 minutes to form a light yellow precipitate. The precipitate was stirred in the mother liquor for 30 minutes. Then, it was filtered and washed 6 times with deionized water. Dry in vacuum at 120°C for 4h. That is to obtain nano solid iron phosphate / PVA / graphene composite material.

[0031] The nanometer solid ferric phosphate / PVA / graphene composite material that present embod...

Embodiment 2

[0035] Graphene oxide was ultrasonically dispersed with deionized water for 30 min to obtain a 1.8 mg / mL suspension. In 100mL deionized water, add 0.1mol Fe(NO 3 ) 3 , 0.1mol (NH 4 ) 2 HPO 4 , 1 g of carbon nanotubes and 1 mL of graphene oxide suspension. The mixture was sonicated in a sonicator for 15 minutes and then placed in a reaction kettle. The continuous stirring speed in the reactor was 100 rad / min. Concentrated ammonia solution was added dropwise to the solution, and the pH value of the mixed solution was adjusted to 3.8. The reaction temperature was kept at 80° C., and the reaction time was 10 h, and a light yellow precipitate was formed. The precipitate was stirred in the mother liquor for 10 hours. Then, filter and wash 3 times with deionized water. Dry in vacuum at 60°C for 20h. That is, the nano solid iron phosphate / carbon nanotube / graphene composite material is obtained.

Embodiment 3

[0037] Graphene oxide was ultrasonically dispersed with deionized water for 60 min to obtain a 3 mg / mL suspension. In 100mL deionized water, add 0.1mol Fe(NO 3 ) 3 , 0.3molH 3 PO 4 , 7 g glucose and 0.3 mL graphene oxide suspension. The mixture was sonicated for 3 minutes in a sonicator and then placed in a reaction kettle. The continuous stirring speed in the reactor was 30rad / min. Concentrated ammonia solution was added dropwise to the solution, and the pH value of the mixed solution was adjusted to 4. The reaction temperature was kept at 120° C., and the reaction time was 5 h, and a light yellow precipitate was formed. The precipitate was stirred in the mother liquor for 5 hours. Then, filter and wash 6 times with absolute ethanol. Dry in vacuum at 85°C for 15h. That is to obtain the nano solid iron phosphate / glucose / graphene composite material.

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Abstract

The invention discloses a nano solid-core iron phosphate-carbon source-graphene composite material; the surfaces of nano solid-core iron phosphate particles are coated with a carbon source, the particles are connected through graphene, and the nano solid-core iron phosphate-carbon source-graphene composite material is formed. The invention also discloses a preparation method of the material. The process flow is simple, the cost is low, at the same time, nitrate radicals are adopted, and the disadvantages in a traditional process that sulfate radicals in an FeSO4 raw material are difficult to wash cleanly and chloride ions in an FeCl3 raw material have a corrosion effect on equipment are overcome. The prepared lithium iron phosphate positive electrode material has the tap density reaching up to 1.68 g/cm<3>, has large volume specific capacity, is beneficial for preparation of a positive electrode material slurry and coating of an electrode slice, and improves the quality of the electrode slice.

Description

technical field [0001] The invention belongs to the technical field of raw material preparation of lithium-ion secondary battery cathode materials, and in particular relates to a nanometer solid iron phosphate-carbon source-graphene composite material and a preparation method thereof. Background technique [0002] Lithium iron phosphate, a cathode material for lithium-ion batteries, has a strong investment value in the energy storage market and the electric market due to its good environmental compatibility, high energy density, long cycle life, high temperature performance and safety performance, such as BYD. Enterprises with a strategic vision have begun to invest in the downstream industry of lithium iron phosphate, have the core technology of "iron battery" using lithium iron phosphate cathode materials, and have accumulated rich industrial experience. [0003] Although lithium iron phosphate has many advantages, due to the crystal structure characteristics of lithium ir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/62B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/364H01M4/5825H01M4/587H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 秦波马锐沈健民宗新林曹炬
Owner 吴位跃
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