Preparation method of three-dimensional graphene structure/high-quality graphene

A graphene and structure technology, applied in the field of materials, can solve the problems of influence, reduction, cycle stability reduction, etc., and achieve the effect of high quality, wide source, and quality improvement

Active Publication Date: 2017-06-23
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many defects on the graphene material sheet obtained by the redox method, and the reduced mechanical, electrical and thermal properties affect its practical application. For example, in energy storage materials, the cycle stability will be reduced.

Method used

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  • Preparation method of three-dimensional graphene structure/high-quality graphene
  • Preparation method of three-dimensional graphene structure/high-quality graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Slowly add 90 ml of concentrated sulfuric acid (98%) to 30 ml of concentrated nitric acid (65%) in an ice-water bath. After mixing evenly, add 3 g of flake graphite (particle diameter 150 microns, containing carbon amount higher than 95%), and stirred at room temperature for 24 hours. Subsequently, the reaction liquid was removed by filtration, and the obtained solid was graphite intercalation compound.

[0028] (2) Slowly add 240ml of concentrated sulfuric acid (98%) into 60ml of hydrogen peroxide (30%) in an ice-water bath, and transfer the mixture into a 40°C water bath after cooling. Subsequently, the graphite intercalation compound in step (1) was added to the mixture, stirred at room temperature for 15 minutes, then allowed to expand for 48 hours, filtered and washed with water to obtain a three-dimensional graphene structure with a specific surface area of ​​1360 m 2 / g, yield 100%. figure 1 The scanning electron microscopy results are given, figure 2 is ...

Embodiment 2

[0031](1) Slowly add 660 ml of concentrated sulfuric acid (98%) to 220 ml of concentrated nitric acid (65%) in an ice-water bath. After mixing evenly, add 3 grams of flake graphite (particle diameter 150 microns, containing carbon amount higher than 95%), and stirred at room temperature for 24 hours. Subsequently, the reaction liquid was removed by filtration, and the obtained solid was graphite intercalation compound.

[0032] (2) Slowly add 240ml of concentrated sulfuric acid (98%) into 60ml of hydrogen peroxide (30%) in an ice-water bath, and transfer the mixture into a 40°C water bath after cooling. Subsequently, the graphite intercalation compound in step (1) was added to the mixed liquid, stirred at room temperature for 15 minutes, then allowed to stand for expansion for 24 hours, washed and filtered to obtain a three-dimensional graphene structure. Specific surface area 1250 m 2 / g, yield 100%.

[0033] (3) Put 0.1 g of wet three-dimensional graphene structure in 100...

Embodiment 3

[0035] (1) Slowly add 90 ml of concentrated sulfuric acid (98%) to 30 ml of concentrated nitric acid (65%) in an ice-water bath. After mixing evenly, add 3 g of flake graphite (particle diameter 500 microns, carbon containing amount higher than 95%), and stirred at room temperature for 24 hours. Subsequently, the reaction solution was suction-filtered with a sand core funnel, and the obtained solid was graphite intercalation compound.

[0036] (2) Slowly add 540ml of concentrated sulfuric acid (98%) into 135ml of hydrogen peroxide (30%) in an ice-water bath, and transfer the mixture into a 40°C water bath after cooling. Subsequently, the graphite intercalation compound in step (1) was added to the mixed liquid, stirred at room temperature for 15 minutes, then allowed to stand for expansion for 3 hours, washed and filtered to obtain a three-dimensional graphene structure. Specific surface area 1320 m 2 / g, yield 100%.

[0037] (3) Put 0.1 g wet three-dimensional graphene str...

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Abstract

The invention provides a preparation method of three-dimensional graphene structure / high-quality graphene. The method comprises the steps of carrying out intercalation treatment on natural flake graphite or synthetic graphite to prepare a graphite intercalation compound; and carrying out expansion treatment on the obtained graphite intercalation compound in an expanding agent to obtain a three-dimensional graphene structure with high specific surface area. A high-quality single-layer or few-layer graphene dispersion liquid is obtained through ball-milling, shearing, high-speed fluid grinding or ultrasonic treatment. The obtained three-dimensional structure has the specific surface area of over 1,000m<2> / g; and the lamellar lattice structure is kept intact. The graphene lattice structure obtained through mechanical exfoliation is kept intact, and has excellent electrical properties; the volume conductivity of a thin film can reach over 1,000S / cm. The prepared graphene material can be widely applied to the fields of energy storage, a composite material, conductive ink, a conductive film and the like. The three-dimensional graphene structure can be directly used as a carbon skeleton with high specific surface area, and can be compounded with various materials such as a polymer, a metal oxide, a metal sulfide and carbon nitride to prepare a composite material with special functionality.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a preparation method of a three-dimensional graphene structure / high-quality graphene, specifically using an oxidizing agent and an acid as an intercalation agent to obtain a graphite intercalation compound; Expanding to obtain a three-dimensional graphene structure; subjecting the obtained three-dimensional structure to physical and mechanical actions such as sand milling, ball milling, shearing, ultrasonic and high-speed fluid pulverization, to obtain a graphene dispersion. Background technique [0002] Due to its unique electronic structure, carbon can form a wide variety of substances through different hybridization methods. Among them, with sp 2 Various carbon nanomaterials (including fullerenes, carbon nanotubes, graphene, etc.) that exist in a hybrid form have become a research hotspot in the field of materials due to their excellent electrical, mechanical, and thermal pro...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B2204/02C01P2002/82C01P2004/03C01P2006/12
Inventor 卢红斌张佳佳赵晓莉李梦雄潘云梅陈宇菲林珊
Owner FUDAN UNIV
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