Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material

A porous spherical, physical method technology, applied in the direction of electrical components, battery electrodes, nanotechnology, etc., can solve the problems of uneven particle size distribution, slow lithium ion diffusion rate, low electronic conductivity, etc., to achieve good electrical conductivity and material Excellent processing performance and uniform particle size distribution

Inactive Publication Date: 2011-04-13
秦波
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  • Application Information

AI Technical Summary

Problems solved by technology

Cathode material LiCoO 2 Already successfully commercialized, but cost prohibitive
LiNiO being extensively studied 2 , LiMn 2 o 4 Cathode materials have their own shortcomings: LiNiO 2 There are security issues, LiMn 2 o 4 The cycle and high temperature performance of LiFePO still need to be greatly improved, and the orthorhombic olivine-type LiFePO as a new lithium-ion battery cathode material 4 It has excellent electrochemical properties and is suitable as a cathode material for lithium-ion secondary batteries
[0004] (1) The electronic conductivity is low, and the diffusion rate of lithium ions in the electrolyte and materials is slow
[0005] (2) Low tap density of the product
[0006] (3) Poor processing performance
[0011] Chinese patent application number CN201010127068.8 discloses a preparation method of porous lithium iron phosphate, which uses high-speed stirring, sand milling or kneading as homogenization treatment means to homogenize raw materials, and essentially only uses physical grinding The method is to grind the raw materials to obtain the primary particles as nano-scale precursors. The nano-scale precursors of primary particles can also be prepared regardless of chemical methods, and the size distribution of primary particles prepared by physical methods is not uniform enough.

Method used

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  • Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material
  • Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material
  • Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material

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Embodiment 1

[0040] Physical method: Weigh 10kg iron phosphate (molecular formula: FePO 4 2H 2 O), in nitrogen (molecular formula: N 2 ) atmosphere, bake at 400°C for 3h to form a dry powder. Get this powder 5Kg, lithium carbonate (molecular formula: Li 2 CO 3 ) 0.9886Kg, dopant magnesium hydroxide (molecular formula: Mg(OH) 2 ) 16g, dopant aluminum oxide 13.5g, add dispersant isopropanol (molecular formula: C 3 h 8 O) 13.9734Kg, forming a slurry. Pore-forming agent citric acid (molecular formula: C 6 h 8 O) 0.0844Kg, stabilizer sodium polystyrene sulfonate (molecular formula: [C 8 h 7 SO 3 Na] n ) 0.0844Kg, coating agent single-wall carbon nanotube 0.0844Kg, add 1Kg isopropanol (molecular formula: C 3 h 8 O), ultrasonically dispersed for 10min, and then poured into the slurry. The above slurry is milled with a stirring ball mill at 400 rad / min for 4 hours, and then sand-milled with a horizontal sand mill at 3800 rad / min for 3.5 hours to form a slurry with primary particles ...

Embodiment 2

[0042] Hydrothermal synthesis method: according to lithium: iron: phosphorus molar ratio is 2: 0.98: 1, weighs 3.97Kg ferrous chloride (molecular formula: FeCl 2 4H 2 0), 0.838Kg lithium hydroxide (molecular formula: LiOH·H 2 O), 1.957Kg phosphoric acid (molecular formula: H 3 PO 4 ), 36g dopant vanadium pentoxide (molecular formula: V 2 o 5 ), add 10.367Kg deoxygenated deionized water (molecular formula: H 2 (0), pH value is 8.67, forms slurry, moves in the autoclave. Coating agent carbon black 0.135Kg, stabilizer cetyltrimethylammonium bromide (molecular formula: C 16 h 33 (CH 3 ) 3 NBr) 0.135Kg, pore forming agent polyvinyl butyral (molecular formula: C 16 h 28 o 5 ) 0.135Kg, put into 8Kg deoxygenated deionized water, ultrasonically disperse for 10min, and put into the slurry. The above high-pressure reaction kettle is a sealed kettle body, nitrogen (molecular formula: N 2 ) protection, the feeding temperature is 80°C, and the stirring speed is 160rad / min. Th...

Embodiment 3

[0045] Co-precipitation method: according to the Li:Fe:P ratio of 2:1:1, ferrous sulfate with a concentration of 110mol / L (molecular formula: FeSO 4 ·7H 2 O), the concentration is 110mol / L ammonium dihydrogen phosphate (molecular formula: NH 4 h 2 PO 4 ) solution and a concentration of 220mol lithium hydroxide (molecular formula: LiOH·H 2 O), the configuration concentration is the NH of 210mol / L 3 ·H 2 O. The mixed solution is added to a certain volume of deoxygenated deionized water (molecular formula: H 2 O) in the reactor, use NH 3 ·H 2 The value of the O adjustment system is 7.0, the temperature of the reaction system is 45° C., and the stirring speed is 120 r / min. A precipitation reaction occurs until the end of the reaction. Nitrogen (N 2 )Protect. Precipitated powder, deoxidized deionized water (molecular formula: H 2 O) Washing to form a slurry. Dopant TiO 2 0.1wt%, pore forming agent polyvinylpyrrolidone (molecular formula: [C 6 h 9 NO] n ) 3wt%, stabi...

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Abstract

The invention discloses a method for preparing a porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material, comprising the specific steps of: dissolving a lithium-containing compound, an iron-containing compound, a phosphor-containing compound and a element-doped compound additive in a dispersing agent to form a sizing agent; dispersing a mixture of a pore-forming agent, a cladding agent and a stabilizer in a dispersing agent through ultrasound, then adding into the sizing agent and mixing to form a new sizing agent; carrying out a physical method or a chemical method on the new sizing agent to obtain a sizing agent with the primary particles in nano grade; carrying out spraying drying and granulating on the obtained sizing agent with the primary particles in nano scale to obtain a dry mixed material with secondary particles with spherical appearances; then carrying out a sintering process on the dry mixed material to obtain the product of the invention. The method has the advantages that besides that the primary particles reach the nano scale, the particle diameters are more uniform in distribution and more regular in appearance, an iron phosphate product synthesized from the material has the particle diameters with uniform distribution, and the material has favorable processability, good electric conductivity, excellent power multiplication performance and higher actual capacity.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material of a lithium ion battery, in particular to a preparation method of a porous spherical lithium ion battery positive electrode material. Background technique [0002] Since 1990, Japan's Sony Corporation has adopted high-potential lithium cobaltate (LiCO) that can reversibly intercalate and deintercalate lithium ions. 2 ) as the positive electrode material, and lithium ion batteries have been developed, and the positive electrode materials for lithium ion batteries have developed rapidly. Cathode material LiCoO 2 It has been successfully commercialized, but the cost is prohibitive. LiNiO being extensively studied 2 , LiMn 2 o 4 Cathode materials have their own shortcomings: LiNiO 2 There are security issues, LiMn 2 o 4 The cycle and high temperature performance of LiFePO still need to be greatly improved, and the orthorhombic olivine-type LiFePO as a new lithium-ion ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/139B82Y40/00
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 秦波孟秦涛
Owner 秦波
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