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A preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene-loaded nickel phosphide material

A phosphorus-doped graphene, lithium-sulfur battery technology, applied in battery electrodes, lithium storage batteries, non-aqueous electrolyte storage batteries, etc., can solve the problems of poor reaction material activity and short positive electrode cycle life, and achieve the effect of suppressing volume expansion

Active Publication Date: 2020-01-14
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the problems of short positive electrode cycle life and poor activity of reactive substances in the prior art, the present invention provides a preparation method of lithium sulfur battery positive electrode material based on phosphorus-doped graphene supported nickel phosphide material

Method used

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  • A preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene-loaded nickel phosphide material
  • A preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene-loaded nickel phosphide material
  • A preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene-loaded nickel phosphide material

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Take 10 mL of 0.2 mg / mL graphene oxide, add 1 mg of hexadecyltrimethylammonium bromide to it, and stir magnetically to obtain a graphene oxide dispersion.

[0024] (2) Add 10mmol of nickel sulfate and 10mmol of sodium hydroxide into 5mL of distilled water, and stir magnetically to obtain a salt solution.

[0025] (3) Slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1) under vigorous stirring, and keep stirring for 5 minutes, then transfer to the reaction kettle, and place in an oven at 140°C After reacting for 6 hours, the obtained product was filtered and freeze-dried to obtain a graphene composite material loaded with nickel precursor.

[0026] (4) Mix the nickel precursor-loaded graphene composite obtained in step (3) with potassium hypophosphite at a mass ratio of 1:1, and calcinate phosphide 1 at a temperature of 250°C in an argon atmosphere tube furnace. hours, phosphorus-doped graphene-supported nickel phosphide material was...

Embodiment 2

[0033] (1) Take 1000 mL of 10 mg / mL graphene oxide, add 200 mg of Triton X100 to it, and stir magnetically to obtain a graphene oxide dispersion.

[0034] (2) Add 1000mmol of nickel hypophosphite and 1000mmol of urea into 50mL of distilled water, and stir magnetically to obtain a salt solution.

[0035] (3) Slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1) under vigorous stirring, and keep stirring for 100 minutes, then transfer to the reaction kettle, and place in an oven at 250°C After reacting for 24 hours, the obtained product was obtained by filtration after the reaction was completed, and freeze-dried to obtain a graphene composite material loaded with nickel precursor.

[0036] (4) Mix the nickel precursor-loaded graphene composite material obtained in step (3) with yellow phosphorus at a mass ratio of 1:50, and calcine phosphating at a temperature of 800 ° C in a helium atmosphere tube furnace for 12 hours , to obtain phosphorus-dop...

Embodiment 3

[0039] (1) Take 20 mL of 5 mg / mL graphene oxide, add 150 mg of polyvinyl alcohol to it, and stir magnetically to obtain a graphene oxide dispersion.

[0040] (2) Add 800mmol of nickel acetate and 40mmol of ammonia water to 30mL of distilled water, and stir magnetically to obtain a salt solution.

[0041](3) Slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1) under vigorous stirring, and keep stirring for 80 minutes, then transfer to the reaction kettle, and place in an oven at 200°C After reacting for 12 hours, the obtained product was filtered and freeze-dried to obtain a graphene composite material loaded with nickel precursor.

[0042] (4) Mix the nickel precursor-loaded graphene composite material obtained in step (3) with sodium hypophosphite at a mass ratio of 1:10, and calcine phosphating at a temperature of 500°C in a nitrogen atmosphere tube furnace for 9 hours , to obtain phosphorus-doped graphene-supported nickel phosphide material...

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Abstract

The invention discloses a preparation method of a lithium-sulfur battery cathode material based on a phosphorus-doped graphene supported nickel phosphide material. The method comprises the following steps: (1) adding a surface active agent into graphene oxide to obtain graphene oxide dispersion liquid; (2) adding a nickel source and alkali liquor into distilled water to obtain a saline solution; (3) adding the saline solution into the graphene oxide dispersion liquid, carrying out a hydrothermal reaction, then washing, and carrying out freeze drying to obtain a graphene composite material loaded with a nickel precursor; (4) enabling the graphene composite material loaded with the nickel precursor to be subjected to a phosphating reaction so as to obtain the phosphorus-doped graphene supported nickel phosphide material; (5) compounding the phosphorus-doped graphene supported nickel phosphide material with sublimed sulfur to obtain the lithium-sulfur battery cathode material based on thephosphorus-doped graphene supported nickel phosphide material. The phosphorus-doped graphene supported nickel phosphide material prepared by the method has a three-dimensional space structure, thus having an obvious domain limiting effect on sulfur and remarkably inhibiting the shuttle effect of lithium polysulfide.

Description

technical field [0001] The invention belongs to the technical field of energy materials, and relates to a preparation method of a lithium-sulfur battery positive electrode material, in particular to a preparation method of a lithium-sulfur battery positive electrode material based on phosphorus-doped graphene-loaded nickel phosphide material. Background technique [0002] The theoretical specific capacity of lithium-sulfur batteries is as high as 2600Wh / kg, which can greatly meet the requirements of electric vehicles for cruising range. At the same time, the characteristics of low pollution and abundant reserves of sulfur make it widely concerned in the field of electrochemical energy storage. However, due to the low intrinsic conductivity of sulfur; the dissolution of lithium polysulfide, an intermediate product of its release point, in the electrolyte; the complex chain scission reaction of long-chain sulfur, and poor electrochemical activity, its development has been rest...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M10/052
CPCH01M4/364H01M4/5805H01M4/583H01M10/052Y02E60/10
Inventor 孙克宁程俊涵张乃庆范立双
Owner HARBIN INST OF TECH
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