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Method for producing lithium transition metal polyanion powders for batteries

Inactive Publication Date: 2010-06-09
CONOCOPHILLIPS CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems include: a) particle aggregation, b) incomplete reaction, c) presence of undesired components in the raw materials and their subsequent presence in the final product, d) poor electrochemical properties of the resulting material, and e) ) require expensive precursors and / or complex processes
Optimum conditions for surface-to-surface contact between particles are often not well achieved as active material particles may be large and / or may be non-uniform in size

Method used

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  • Method for producing lithium transition metal polyanion powders for batteries
  • Method for producing lithium transition metal polyanion powders for batteries
  • Method for producing lithium transition metal polyanion powders for batteries

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Embodiment 1: the LVP powder of the present invention is prepared as follows: 30.68 grams of vanadium trioxide powder (V 2 o 3 , 95%) and 100 ml of NMP (1-methyl-2-pyrrolidone) were placed in a grinding vial and ball milled for about 30 minutes using about 1 pound of 1 / 4" stainless steel balls. In a glass beaker, 59.575 grams of acetic acid Lithium dihydrate (LiC 2 h 3 o 2 2H 2 O, 99.9%) and 78.61 grams of diammonium phosphate ((NH 4 ) 2 HPO 4 , 98%) was dissolved in 100ml of water. will V 2 o 3 Suspension and LiC 2 h 3 o 2 2H 2 O / (NH 4 ) 2 HPO 4 / water solution were combined in a glass flask and an additional 500 ml NMP was added to the suspension. The suspension was heated at the boiling point with constant stirring and purged with nitrogen until all solvents (NMP and water) were completely evaporated. The resulting product is a flowable powder.

[0074] The LVP powder was placed in an alumina boat and heated in a tube furnace under a nitrogen atmos...

Embodiment 2

[0075]Example 2 uses LVP powder produced by the method described in Example 1 and coats the powder with 2.6% by weight of pitch using petroleum pitch as a precursor. Dissolve 2 grams of petroleum pitch in approximately 4 grams of xylene and heat to 90°C. A suspension consisting of 7.6 g of LVP powder in 200 g of xylene was heated to 140°C. The bitumen / xylene solution was added to the powder / xylene suspension and stirring was continued for 10 minutes. The heater was then removed to allow the suspension to cool to room temperature. The resulting solid powder was isolated by filtration and dried under vacuum at 100°C. The resulting powder weighed 8 grams. The bituminous coating constitutes about 2.6% by weight. The pitch-coated powder was placed in a tube furnace and gradually heated to 300°C at a rate of 1°C / min in a nitrogen atmosphere and kept at 300°C for 6 hours. The tube furnace was cooled to ambient temperature and the powder was removed and blended in plastic bottles...

Embodiment 3

[0076] Example 3 used the LVP powder produced by the method described in Example 1 and coated the powder with 2.3% by weight of pitch using the same pitch as in Example 2 as a precursor. 7 grams of bitumen were dissolved in approximately 7 grams of xylene and heated to 90°C. A suspension consisting of 30 g of LVP powder in 200 g of xylene was heated to 140°C. The bitumen / xylene solution was added to the powder / xylene suspension and stirring was continued for 10 minutes. The heater was then removed to allow the suspension to cool to room temperature. The resulting solid powder was isolated by filtration and dried under vacuum at 100°C. The resulting powder weighed 30.8 grams. The bituminous coating constitutes about 2.6% by weight. The pitch-coated powder was placed in a tube furnace and gradually heated to 300°C at a rate of 1°C / min in a nitrogen atmosphere and kept at 300°C for 6 hours. The tube furnace was cooled to ambient temperature and the powder was removed and ble...

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Abstract

This invention relates to a process for producing an improved powder for the positive electrode of lithium ion batteries wherein the powder comprises lithium, vanadium and phosphate. The process includes forming a suspension of the precursors with a high boiling temperature solvent and heating the suspension to a reaction temperature of between 250 DEG C and 400 DEG C to convert the precursors to the desired solid product. The solid product is separated from the suspension and is heated to a higher temperature to crystallize the product. The resulting product retains a small particle size thus avoiding the need for milling or other processing to reduce the product to a particle size suited for batteries.

Description

[0001] Statement Regarding Research or Development Sponsored by the Federal Government [0002] none technical field [0003] The present invention relates to materials for positive electrodes of lithium-ion batteries and methods of making such materials. Background technique [0004] Lithium-ion battery packs are recognized and valued for their high efficiency, energy density, high cell voltage, and long shelf life, and have been in commercial use since the early 1990s. Though as always, there is still a desire to make better battery packs at a lower cost. [0005] A key component of current lithium-ion batteries is lithium transition metal polyanion salt powder, which is provided as the active material on the positive metal plate. Iron, cobalt, manganese and nickel powders have been used and other transition metals have been considered. Cobalt has high performance, but has proven to be unsafe as it could cause an explosion during recharging. Iron is attractive because ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/30C01G53/00H01M4/58H01M4/136H01M10/052H01M10/36
CPCC01B25/45H01M4/5825H01M4/625H01B1/122H01M2300/004H01M4/136H01M10/052H01M4/366Y02E60/12Y02E60/10
Inventor 毛振华
Owner CONOCOPHILLIPS CO