Preparation method of three-dimensional graphene-based foam material

A graphene-based and foamed material technology is applied to the preparation of graphene materials and the preparation of three-dimensional graphene-based foams, and can solve the problems of reduced application performance, difficulty in reaching the lowest density, low cleanliness of three-dimensional graphene, etc. easy effect

Active Publication Date: 2015-03-11
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] One of the main difficulties in the preparation of three-dimensional graphene materials is that the graphene sheets are aggregated with each other, making it difficult to achieve the lowest density, which in turn limits its performance and application range.
Although the hydrothermal method can realize the large-scale production of three-dimensional graphene, the cleanliness of the synthesized three-dimensional graphene is not high and is accompanied by the agglomeration of graphene sheets, and the structure is easy to collapse, which reduces its application performance; while the growth conditions of the CVD method are harsh , it is difficult to achieve mass production of three-dimensional graphene
[0004] The present invention proposes a preparation method of a three-dimensional graphene-based foam, which can overcome existing problems. At present, domestic and foreign publications and patents have not yet been reported.

Method used

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  • Preparation method of three-dimensional graphene-based foam material
  • Preparation method of three-dimensional graphene-based foam material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of graphene oxide:

[0019] First, add 50 mL of concentrated sulfuric acid (92 g) to a round bottom flask, heat it to a temperature of 80-90°C in an oil bath, then add 10 g of potassium persulfate and 10 g of phosphorus pentoxide, and then add 10 g of natural stone The ink powder was slowly added and kept for 4 hours. After cooling to room temperature, the mixture was diluted with deionized water, then vacuum filtered, washed with 3 L of deionized water, and the solid was dried under vacuum for more than one day, and finally the preoxidized Graphite powder; secondly, in a 2L beaker, add 230 mL (4.3 mol) of concentrated sulfuric acid, cool to 0°C, then add 5 g (0.42 mol) of pre-oxidized graphite powder in the first step, and then add 30 g (0.19 mol) of high Potassium manganate was added to the beaker in batches while keeping the temperature below 10°C, and then kept in a water bath at a temperature of 38°C for 2 hours for the optimal time, then diluted with 0...

Embodiment 2

[0024] Prepare graphene oxide and carry out by embodiment 1;

[0025] Disperse the obtained graphene oxide product into 20mL furfuryl alcohol solution to form a graphene oxide-furfuryl alcohol solution with a concentration of 4 mg / mL, ultrasonically disperse to form a uniform graphene oxide-furfuryl alcohol mixture, then add oxalic acid and stir evenly, wherein oxalic acid and The molar ratio of furfuryl alcohol solution is 0.09:1;

[0026] Immerse the polymer foamed polyethylene foam in the obtained furfuryl alcohol solution for 0.5 hours, then squeeze the foam evenly, and then polymerize and cure it in an oven at a temperature of 100°C for 2 hours to obtain a cured polymer foam;

[0027] Put the cured composite foam in a quartz boat, slowly raise the temperature to 900 °C at 2 °C / min in a tube furnace under argon gas, keep it warm for 2 hours, and naturally cool to room temperature to obtain three-dimensional graphene base foam;

[0028] In a Petri dish filled with water, ...

Embodiment 3

[0030] Prepare graphene oxide and carry out by embodiment 1;

[0031] Disperse the obtained graphene oxide product into 20mL furfuryl alcohol solution to form a graphene oxide-furfuryl alcohol solution with a concentration of 6 mg / mL, ultrasonically disperse to form a uniform graphene oxide-furfuryl alcohol mixture, then add oxalic acid and stir evenly, wherein oxalic acid and The molar ratio of furfuryl alcohol solution is 0.13:1;

[0032] Immerse the polymer foamed polyvinyl chloride foam in the obtained furfuryl alcohol solution for 0.5 hours, squeeze the foam evenly, and polymerize and cure it in an oven at a temperature of 120°C for 3 hours to obtain a cured composite foam;

[0033] The cured composite foam was slowly heated up to 950°C at a temperature of 4°C / min in a nitrogen environment, kept for 4 hours for heat treatment, and cooled naturally to room temperature to obtain a three-dimensional graphene-based foam material.

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Abstract

The invention relates to a preparation method of a three-dimensional graphene-based foam material, which comprises the steps of stripping graphite to obtain graphite oxide with an improved Hummers method, taking graphite oxide with dispersed furfuryl alcohol as a carbon source and a high polymer foam material as a template, obtaining a high polymer foam material obtaining graphite oxide with a simple impregnation method, and obtaining the three-dimensional graphene-based foam material by heat treatment of high polymer foam under an anaerobic condition. The three-dimensional graphene-based foam material prepared by the method is provided with a graphene-based foam macro body in a three-dimensional continuous structure; the method is easy and simple to operate, and high in productivity; a foam structure is easy to adjust and control; the prepared three-dimensional graphene-based foam material has the advantages of high electroconductivity, large specific surface area, lipophilicity, hydrophobicity and the like; and a foundation is laid for the application of the three-dimensional graphene-based foam material in the fields of heat-conducting composites, catalytical materials, energy storage materials, phase separation materials, adsorbing materials and the like.

Description

technical field [0001] The invention relates to a method for preparing a graphene material, in particular to a method for preparing a three-dimensional graphene-based foam, and belongs to the field of functional materials. Background technique [0002] Graphene is a two-dimensional honeycomb crystal structure formed by densely packing a single layer of carbon atoms, and is the basic structural unit for constructing other dimensional carbon materials (such as zero-dimensional fullerene, one-dimensional carbon nanotubes, and three-dimensional graphite). The unique crystal structure of graphene makes it have excellent electrical, thermal and mechanical properties. Single-layer graphene can be used in field-effect transistors, high-frequency devices, super microprocessors and single-molecule detectors. The three-dimensional structure composed of graphene as the basic unit, such as bulk materials or thin films, may be applied in controllable gas-permeable membranes, anisotropic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 杨苏东马鹏程陈琳王传义
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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