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Three-dimensional graphene material with microporous-mesoporous-macroporous hierarchical structure and its preparation method and application

A technology of graphene and graphene layers, which is applied in the field of three-dimensional graphene materials and its preparation, can solve the problems affecting the comprehensive performance of three-dimensional graphene skeleton composite materials, easy residue of polymers, complex preparation process, etc., and achieve controllable pore size distribution , easy process and simple process

Active Publication Date: 2018-09-28
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the electrical performance has been improved, before this method removes the template, it is necessary to deposit a layer of polymer PMMA for protection and support. After removing the template, it is necessary to use an organic solvent to remove the support material. The preparation process is complicated, and the polymer is easy to remain. This will seriously Affecting the Comprehensive Properties of Three-dimensional Graphene Framework Composites
This three-dimensional graphene has a large pore structure (~hundreds of microns), resulting in poor mechanical strength and low surface area, and the specific capacity of the supercapacitor is only 4.7F / g (Y.He, W.Chen, X.Li , Z. Zhang, J. Fu, C. Zhao, E. Xie, ACS Nano 2013, 7, 174.)

Method used

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  • Three-dimensional graphene material with microporous-mesoporous-macroporous hierarchical structure and its preparation method and application
  • Three-dimensional graphene material with microporous-mesoporous-macroporous hierarchical structure and its preparation method and application
  • Three-dimensional graphene material with microporous-mesoporous-macroporous hierarchical structure and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Utilize sol-gel method to prepare porous silica template (New J.Chem.,2007,31,1907), its photo is as follows figure 2 shown. Use it as a reaction substrate, put it into a chemical vapor deposition reaction furnace, heat it to a reaction temperature of 1100°C and keep the temperature constant for 10 minutes, then introduce methane, hydrogen and argon, and their gas flow rates are 20, 50 and 500 sccm (ml / min) respectively , carry out chemical vapor deposition reaction, the reaction time is 60min; the composite substrate with graphene growth is placed in 10% hydrofluoric acid and 15% hydrochloric acid etching solution, and the template is removed; after vacuum drying in ethanol, three-dimensional graphite is obtained alkene material, whose photo is shown in image 3 shown. 3D graphene exhibits a porous hierarchical structure ( Figure 4a , 4b ), the number of graphene layers is 1-3 ( Figure 5 ), the conductivity is 35S / cm, and the specific surface area is 1580m 2 / ...

Embodiment 2

[0060] Change the chemical vapor deposition reaction time in Example 1 to 120min; put the composite substrate grown with graphene into 15% hydrofluoric acid and 25% hydrochloric acid etching solution, remove the template; carry out freeze-drying to obtain a three-dimensional Graphene material, the number of graphene layers is 3-7, the electrical conductivity is 55S / cm, and the specific surface area is 1280m 2 / g( Image 6 ), the specific capacity of the supercapacitor is 286F / g.

Embodiment 3

[0062] The porous alumina used in Example 1 was used as a template, placed in a chemical vapor deposition reaction furnace, heated to a reaction temperature of 800°C and kept at a constant temperature for 5 minutes, then introduced propane, ammonia, hydrogen and argon, and their gas flow rates were 50, 200, 300 and 600sccm (milliliters / minute), carry out chemical vapor deposition reaction, reaction time 120min; Put the composite substrate that grows graphene into 8% hydrofluoric acid and 15% phosphoric acid etching solution, remove template; Carry out Freeze drying to obtain a nitrogen-doped three-dimensional graphene material with a nitrogen content of 3.8%. The number of graphene layers is 2-8. The conductivity is 65S / cm, and the specific surface area is 2380m 2 / g, the specific capacity of the supercapacitor is 425F / g.

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Abstract

The invention relates to a three-dimensional graphene material with a microporous-mesoporous-macroporous multistage structure and a preparation method and an application of the three-dimensional graphene material. The three-dimensional graphene material has the microporous-mesoporous-macroporous multistage structure; graphene layers are 1-10 atom layers; the specific surface area of the three-dimensional graphene material is 500-3500m<2> / g, and the conductivity is 10-300S / cm; and the three-dimensional graphene material is a block material on a macro scale. The three-dimensional graphene material with the microporous-mesoporous-macroporous multistage structure has the advantages of low cost, high conductivity (the conductivity is 10-300S / cm) and large specific surface area (500-3500m<2> / g).

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a three-dimensional graphene material with a microporous-mesoporous-macroporous multi-level structure and a preparation method thereof, which are mainly used in the fields of supercapacitors, photovoltaics, semiconductor electronics, and composite materials. Background technique [0002] Graphene is a two-dimensional (2D) periodic honeycomb lattice structure composed of carbon six-membered rings, which is the basis for constructing other dimensional carbon-based materials (0D fullerenes, 1D carbon nanotubes and 3D graphite). unit. The unique crystal structure of graphene endows it with excellent properties, such as high thermal conductivity, high mechanical strength, and peculiar electrical and optical properties. Graphene powder has a large specific surface area (such as the graphene powder disclosed in the patent application No. 201510018915.X), which is easy to agglomerate and st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/186B82Y40/00H01G11/36
CPCY02E60/13
Inventor 黄富强毕辉
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI