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Preparation method of lithium vanadium phosphate/graphene/carbon composite positive electrode material

A composite cathode material, lithium vanadium phosphate technology, applied in battery electrodes, electrical components, electrochemical generators, etc., can solve the problems of affected product performance, poor concentration control, cumbersome operation, etc. The effect of superior performance and simple process

Active Publication Date: 2018-02-16
郴州博太超细石墨股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Combining the two, there is no method for preparing lithium iron phosphate / graphene / carbon composite materials. Fudan University used ethylene glycol as a solvent to synthesize lithium iron phosphate / graphene / carbon composites in situ at 250°C by solvothermal method. Materials, through this method can be synthesized to obtain nano-sized lithium iron phosphate particles with better uniformity, and make the lithium iron phosphate particles evenly distributed on the graphene sheet, so that graphene can provide lithium ion migration channels, while ethylene two Alcohol can improve the dispersion of lithium iron phosphate particles, but the method is cumbersome to operate, the cost is high, the concentration is not easy to control, and the product performance is affected. At the same time, this method is not suitable for the preparation of lithium vanadium phosphate / graphene / carbon composite Material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] V on the surface 2 o 5 Preparation of the matrix: the V 2 o 5 Dissolve in pure water to prepare 0.1 mmol / ml V 2 o 5 Spray evenly on the wood butterfly substrate with a simple spray device, then put the stainless steel substrate in a vacuum drying oven at 80°C for 4 hours, then place the wood butterfly substrate in a tube furnace, in a nitrogen atmosphere, Calcined at 300°C for 2 hours to obtain V on the surface 2 o 5 wooden butterfly substrate.

[0030] S1. Dissolve lithium acetate, vanadium pentoxide and ammonium dihydrogen phosphate with a molar ratio of 3:1:3 in deionized water, then add 5% sodium citrate and 5% graphene oxide, and place under magnetic stirring Stir at 70°C for 0.5h to form a mixed solution;

[0031] S2, lay the substrate with vanadium pentoxide on the surface and place it in the mixed solution obtained in step S1 for immersion for 3 days, take out the substrate after impregnation and place it in a vacuum drying oven to dry, then put it in a ...

Embodiment 2

[0036] V on the surface 2 o 5 Preparation of the matrix: the V 2 o 5 Dissolve in pure water to prepare 0.1 mmol / ml V 2 o 5 The aqueous solution of the rush grass is evenly sprayed on the rush grass substrate with a simple spray device, and then the rush grass substrate is placed in a vacuum drying oven at 80 ° C for 5 hours, and then the rush grass substrate is placed in a tube furnace, in a nitrogen atmosphere , Calcined at 300°C for 8 hours, the surface has V 2 o 5 The rush substrate.

[0037]S1. Dissolve lithium acetate, vanadium pentoxide and ammonium dihydrogen phosphate with a molar ratio of 3:1:3 in deionized water, then add 10% sodium citrate and 7% graphene oxide, and place under magnetic stirring Stir at 80°C for 0.5h to form a mixed solution;

[0038] S2, lay the substrate with vanadium pentoxide on the surface and place it in the mixed solution obtained in step S1 for immersion for 4 days, take out the substrate after impregnation and place it in a vacuum d...

Embodiment 3

[0043] V on the surface 2 o 5 Preparation of the matrix: the V 2 o 5 Dissolve in pure water to prepare 0.1 mmol / ml V 2 o 5 The aqueous solution of the rush grass is evenly sprayed on the rush grass substrate with a simple spray device, and then the rush grass substrate is placed in a vacuum drying oven at 120 ° C for 1 hour, and then the rush grass substrate is placed in a tube furnace, in a nitrogen atmosphere , Calcined at 400°C for 1 hour to obtain V on the surface 2 o 5 The rush substrate.

[0044] S1. Dissolve lithium acetate, vanadium pentoxide and ammonium dihydrogen phosphate with a molar ratio of 3:1:3 in deionized water, then add 15% sodium citrate and 8% graphene oxide, and place under magnetic stirring Stir at 80°C for 0.5h to form a mixed solution;

[0045] S2, lay the substrate with vanadium pentoxide on the surface and place it in the mixed solution obtained in step S1 for immersion for 5 days, take out the substrate after impregnation and place it in a ...

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Abstract

The invention specifically relates to a preparation method of a lithium vanadium phosphate / graphene / carbon composite positive electrode material. The preparation method comprises the steps of adding asoluble lithium compound, vanadium compound and phosphate into deionized water based on an appropriate proportion to prepare a solution; next, adding a proper amount of sodium citrate and graphene oxide; then putting a carbon substrate, the surface of which is attached with the vanadium compound, into the mixed solution in a horizontal manner to be immersed for several days, next, taking the immersed carbon substrate out and drying the substrate, and performing high-temperature calcining in protection atmosphere for a certain time, and then taking the product out and performing cooling; and repeatedly executing the above steps and finally performing low-temperature carbonization treatment and high-temperature synthesis treatment in sequence to obtain the lithium vanadium phosphate / graphene / carbon composite positive electrode material on the surface of the substrate. The lithium vanadium phosphate positive electrode material not only has the advantages of high specific capacity, high cycle performance, high rate capability and the like, but also combines the advantages of the low cost, green environmental protection and the like.

Description

technical field [0001] The invention belongs to the technical field of battery positive electrode composite materials, and more specifically relates to a preparation method of lithium vanadium phosphate / graphene / carbon composite positive electrode material. Background technique [0002] Since Goodenough et al first proposed the lithium iron phosphate polyanionic lithium battery positive electrode material, researchers have carried out a lot of research on polyanionic phosphate, the most successful of which is the industrial production of lithium iron phosphate positive electrode material. There are not many research reports, and industrial production has not yet been realized. However, lithium vanadium phosphate is a material with better performance than lithium iron phosphate, and has the following advantages: a. It has excellent thermal stability, which is only slightly lower than lithium iron phosphate in the positive electrode materials currently being studied; b. There...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/364H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 林荣铨
Owner 郴州博太超细石墨股份有限公司
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