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Preparation method for nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate

A lithium-ion battery, lithium vanadium fluorophosphate technology, applied in battery electrodes, nanotechnology, nanotechnology and other directions, can solve the problems of low electronic conductivity, limit high-rate discharge performance, etc., and achieve high specific surface area and excellent electrochemical performance. , is conducive to the effect of embedding and detachment

Active Publication Date: 2014-06-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] LiVPO 4 F has a three-dimensional frame structure, which greatly improves its ionic conductivity, but its low electronic conductivity severely limits its high-rate discharge performance

Method used

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  • Preparation method for nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate
  • Preparation method for nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate
  • Preparation method for nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 0.91 g of vanadium pentoxide, 1.15 g of diammonium hydrogen phosphate, and 1.4 g of citric acid, dissolve them in 50 mL of deionized water; stir in a water bath at 80°C for 4 hours to form a uniform blue solution; adjust the pH of the solution to 7 with ammonia water ; Transfer the solution to a polytetrafluoroethylene tank, place the polytetrafluoroethylene tank containing the solution in a pyrolysis tank, heat and react at 250°C for 20h, cool naturally to room temperature, and take out the reaction product; filter, and filter the product Dry in a vacuum oven at 80°C to obtain an amorphous vanadium phosphate precursor; grind the dried amorphous vanadium phosphate precursor in an agate mortar, then place it in a tubular sintering furnace, sintering at 700°C for 6 h, and then naturally cooled to room temperature to obtain a crystalline vanadium phosphate precursor; weigh 0.438 g of crystalline vanadium phosphate precursor and 0.078 g of lithium fluoride, and grind t...

Embodiment 2

[0038] Weigh 1.82g of vanadium pentoxide, 2.3g of diammonium hydrogen phosphate, and 4.4g of oxalic acid, and dissolve them in 80mL of deionized water; stir in a water bath at 80°C for 2 hours to form a uniform green solution; adjust the pH of the solution to 2 with ammonia water; The solution was transferred to a polytetrafluoroethylene tank, and the polytetrafluoroethylene tank containing the solution was placed in a pyrolysis tank, heated and reacted at 280°C for 18 hours, cooled to room temperature, and the reaction product was taken out; filtered, and the filtered product was placed in a vacuum oven Dry at 80°C to obtain an amorphous vanadium phosphate precursor; grind the amorphous vanadium phosphate precursor in an agate mortar, then place it in a tube sintering furnace, and sinter at 600°C for 2 hours in an argon atmosphere , and then naturally cooled to room temperature to obtain a crystalline vanadium phosphate precursor; weigh 0.438g of vanadium phosphate precursor, ...

Embodiment 3

[0041] Weigh 1.17g of ammonium metavanadate, 1.15g of diammonium hydrogen phosphate, and 1.4g of citric acid, and dissolve them in 80mL of deionized water; stir in a water bath at 80°C for 6 hours to form a uniform green solution; adjust the pH of the solution to 12 with ammonia water; Transfer the solution to a polytetrafluoroethylene tank, place the polytetrafluoroethylene tank containing the solution in a pyrolysis tank, heat and react at 230°C for 25 hours, cool to room temperature, and take out the reaction product; filter, and put the filtered product in a vacuum Dry in an oven at 80°C to obtain an amorphous vanadium phosphate precursor; grind the amorphous vanadium phosphate precursor in an agate mortar, then place it in a tube sintering furnace, and sinter it at 725°C under an argon atmosphere 8h, then cool down to room temperature naturally to obtain the vanadium phosphate precursor; weigh 0.438g of the vanadium phosphate precursor, 0.126g of sodium fluoride, and 0.11g...

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Abstract

The invention provides a preparation method for a nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate. The preparation method comprises the following step: (1) dissolving a vanadium source, a phosphorus source and a reducing agent into water; (2) agitating in a water bath; (3) adjusting the pH to 2-12; (4) transferring the solution to a polytetrafluoroethylene tank; putting the polytetrafluoroethylene tank into a pyrolysis tank, and heating and reacting at 220-280 DEG C for 15-25 hours; cooling to a room temperature; (5) filtering and drying in vacuum; (6) arranging into an agate mortar to be grinded; then sintering under a non-oxidization atmosphere; cooling to the room temperature to obtain a crystallized-state vanadium phosphate precursor; (7) mixing the crystallized-state vanadium phosphate precursor with a lithium source and a fluorine source; uniformly grinding; and (8) arranging a mixture into a pipe type sintering furnace and sintering under the non-oxidization atmosphere; and cooling to the room temperature to obtain the nano sheet-shaped lithium ion battery positive electrode material fluorine lithium vanadium phosphate. According to the preparation method, the microcosmic appearance of the positive electrode material is in a sheet-shaped structure with the thickness being in a nano grade; the surface of a nano sheet is uniformly coated with carbon and the appearance of the material is special; the excellent electrochemical performance is represented.

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 lithium vanadium phosphate, a positive electrode material of a nano-sheet lithium ion battery. Background technique [0002] Lithium vanadium fluorophosphate (LiVPO 4 F) is a new type of lithium-ion battery cathode material, which passes VO 4 f 2 The intersection of the octahedral corners allows the chain to be extended, by sharing the PO 4 The corners of the tetrahedron make the chains intersect to form a three-dimensional network structure in space, and there are two crystallization positions where lithium ions can be intercalated, so it has excellent charge and discharge performance and high rate performance. LiVPO 4 The oxygen ion of F is covalently bonded to P 5+ Formation (PO 4 ) 3- Polyanionic groups, thereby ensuring the stability of oxygen in the lattice, are more stable than traditional two-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCB82Y30/00H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 郑俊超韩亚东张宝袁新波欧星王小玮
Owner CENT SOUTH UNIV
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