Preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene supported nickel phosphide material

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

Active Publication Date: 2018-02-06
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 invent

Method used

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  • Preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene supported nickel phosphide material
  • Preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene supported nickel phosphide material
  • Preparation method of lithium-sulfur battery cathode material based on phosphorus-doped graphene supported nickel phosphide material

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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 cetyltrimethylammonium bromide to it, and stir magnetically to obtain a graphene oxide dispersion.

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

[0025] (3) Under vigorous stirring, slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1), and continue to stir for 5 minutes, and then transfer to the reactor, in an oven at 140°C After reacting for 6 hours, the product obtained after the reaction is obtained by filtration and freeze-dried to obtain a graphene composite material supporting the nickel precursor.

[0026] (4) The nickel precursor-loaded graphene composite material obtained in step (3) is mixed with potassium hypophosphite in a mass ratio of 1:1, and the phosphating 1 is calcined in an argon atmosphere tube furnace at a temperature of 250°C. After hours, phosphorus-doped graph...

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 1000 mmol of nickel hypophosphite and 1000 mmol of urea to 50 mL of distilled water, and magnetically stir to obtain a salt solution.

[0035] (3) Under vigorous stirring, slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1), and continue to stir for 100 minutes, and then transfer to the reactor, in an oven at 250°C After reacting for 24 hours, the product obtained after the reaction is filtered and freeze-dried to obtain a graphene composite material supporting the nickel precursor.

[0036] (4) The nickel precursor-loaded graphene composite material obtained in step (3) is mixed with yellow phosphorus in a mass ratio of 1:50, and phosphating is calcined in a helium atmosphere tube furnace at a temperature of 800°C for 12 hours , To obtain phosphorus-doped graphene supported nickel phosphi...

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 800 mmol of nickel acetate and 40 mmol of ammonia to 30 mL of distilled water, and magnetically stir to obtain a salt solution.

[0041] (3) Under vigorous stirring, slowly add the salt solution in step (2) to the graphene oxide dispersion in step (1), and continue stirring for 80 minutes, then transfer to the reactor, and place it in an oven at 200°C. After reacting for 12 hours, the product obtained after the reaction is filtered and freeze-dried to obtain the graphene composite material supporting the nickel precursor.

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

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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 rich 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 have been restricting its development. ...

Claims

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Application Information

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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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