A preparation method of a sulfur-supported graphene aerogel composite material

A technology of graphene airgel and composite materials, which is applied in the field of preparation of graphene airgel-supported sulfur composite materials, and can solve the problems of poor cycle stability of lithium-sulfur batteries, poor cycle stability of batteries, and reduced utilization of sulfur and other problems, to achieve the effect of short preparation cycle, improved electrochemical performance and large output

Inactive Publication Date: 2014-08-20
SHANGHAI UNIV
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Problems solved by technology

The generation of the shuttle effect directly leads to the reduction of sulfur utilization rate and the corrosion of lithium negative electrode, which makes the battery cycle stability worse and the coulombic efficiency lower
In addition, the conductivity of sulfur is extremely low (at 25°C, Ω = 5 × 10-30 S / cm), and insoluble Li2S is deposited on the negative electrode during charge and discharge. , dendrites are formed on the lithium negative electrode, and the volume expansion and fragmentation of the S positive electrode will cause the cycle stability of the lithium-sulfur battery to deteriorate.

Method used

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  • A preparation method of a sulfur-supported graphene aerogel composite material
  • A preparation method of a sulfur-supported graphene aerogel composite material
  • A preparation method of a sulfur-supported graphene aerogel composite material

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Embodiment 1

[0032] One, prepare graphene oxide with traditional known process

[0033] Potassium persulfate (K 2 S 2 o 8 ) 2.5 g, phosphorus pentoxide (P 2 o 5 ) 2.5 g, dissolved in 12 mL of concentrated sulfuric acid, heated to 80°C; then 3 g of natural graphite was added to the above solution, kept at 80°C for 4.5 hours; cooled to room temperature, diluted with 500 mL of deionized water, and left standing overnight ; filter, float residual acid with 0.2 mm filter; dry in a vacuum oven at 60°C; add the obtained preoxide to 120 mL of ice-bathed concentrated sulfuric acid, slowly add 15 g of KMnO under stirring 4 , Keep the temperature below 20°C during the addition process. Then the temperature was controlled at 35°C and stirred for 2 h. Add 250 mL of deionized water to dilute, and keep the temperature below 50°C in an ice bath during the dilution process. Stir for another 2 h, add 0.7 L of deionized water, and immediately add 20 mL of 30% H 2 o 2 , the mixture produced bubbles, ...

Embodiment 2

[0042] The preparation method of graphene oxide is the same as above-mentioned embodiment 1.

[0043] 1) Disperse 80 mg of graphene oxide in 50 mL of deionized water, sonicate for 24 h; add 5 mL of isopropanol solution, stir for 5 h; add 3 mL of sulfur / carbon disulfide solution with a mass-volume ratio of 75 mg / mL , stirred for 1.5 h; the solution was transferred to a reaction kettle, kept at a constant temperature for 48 h at 100 °C, soaked in alcohol and deionized water three times, frozen and sectioned, and dried to obtain a composite material of graphene airgel loaded with sulfur ;

[0044] 2) Immerse the graphene airgel composite material in a solution of 0.1 mol / L pyrrole monomer and 1 mol / L hydrochloric acid for 0.5 h; place the soaked material on a watch glass, add potassium permanganate dropwise, and react After 24 h, the polypyrrole-coated graphene airgel-loaded sulfur composite was obtained.

Embodiment 3

[0046] The preparation of graphene oxide is the same as above-mentioned embodiment 1.

[0047] 1) Disperse 200 mg of graphene oxide in 50 mL of deionized water, sonicate for 12 h; add 25 mL of absolute ethanol solution, stir for 2 h; add 3 mL of sulfur / carbon disulfide solution with a mass-volume ratio of 100 mg / mL , stirred for 1.5 h; the solution was transferred to the reactor, kept at a constant temperature of 150 °C for 24 h, soaked in alcohol and deionized water three times respectively, frozen and sectioned, and dried to obtain a composite material of graphene airgel loaded with sulfur ;

[0048] 2) Immerse the graphene airgel composite material in a solution of 0.5 mol / L aniline monomer and 1 mol / L hydrochloric acid for 0.5 h; place the soaked material on a watch glass, add potassium dichromate dropwise, and react for 24 h Obtained polyaniline-coated graphene airgel-loaded sulfur composites.

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Abstract

The invention relates to a preparation method of a sulfur-supported graphene aerogel composite material, and belongs to the technical field of lithium ion battery cathode materials. The preparation method mainly includes steps of: subjecting a graphene oxide dispersion liquid, ethanol and sulfur / carbon disulfide which are main raw materials to a hydrothermal reaction at 100-200 DEG C for 6-48 h to obtain sulfur-supported graphene aerogel, and obtaining the sulfur-supported graphene aerogel composite material covered by a polymer through a chemical oxidation method. According to a sulfur-supported graphene aerogel cathode prepared by the preparation method, graphene is staggered and connected to form a three-dimensional conductive network, the supramaximal surface area can absorb more sulfur, and covering by the polymer can overcome a problem of volume expansion of sulphur and a problem of material smashing in charge-discharge processes. In addition, the composite material prepared by the preparation method can be directly used as a pole piece, thus omitting tedious processes, such as pulping and coating in traditional electrode preparation. The preparation method is prone to industrial production.

Description

technical field [0001] The invention relates to a preparation method of a graphene airgel-supported sulfur composite material, which belongs to the field of lithium-ion battery electrode material manufacturing. Background technique [0002] Due to the advantages of high working voltage, high energy density (light weight), no memory effect, long cycle life and no pollution, lithium-ion secondary batteries have become the preferred power source for various electronic products in recent years. However, with the advent of the mobile Internet era, the miniaturization of electronic equipment, and the large-scale development and application of electric bicycles, electric vehicles, and large-scale energy storage power stations, higher specific capacity requirements have been put forward for lithium-ion secondary batteries. [0003] In the lithium-ion secondary battery system, compared with negative electrode materials (such as graphite and silicon negative electrode materials, the t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/38H01M4/58H01M4/62
CPCH01M4/364H01M4/625H01M10/0525Y02E60/10
Inventor 蒋永赵兵凌学韬王志轩陈卢陆孟娜陈勇焦正吴明红
Owner SHANGHAI UNIV
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