Preparation method of high-conductivity and high-elasticity three-dimensional graphene material

A graphene, high-elasticity technology, applied in the direction of graphene, chemical instruments and methods, nano-carbon, etc., can solve problems that are not suitable for large-scale manufacturing, expensive equipment and energy, graphene oxide removal, etc., to improve mechanics and electricity Performance, improvement of reduction degree, effect of preventing volume expansion

Active Publication Date: 2021-10-12
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, ethylenediamine is used as a chemical reducing agent to construct a three-dimensional graphene structure. The epoxy group of ethylenediamine undergoes a nucleophilic ring-opening reaction on the surface of graphene oxide, resulting in effective self-assembly[1], but its mechanical properties are insufficient: the yield stress is 5.9kPa, and the maximum reversible elastic strain is 80%
The experimental conditions of high temperature and high pressure not only require expensive equipment and energy, but also are not suitable for large-scale manufacturing
At the same time, there is an existing problem that the hydrothermal chemical reduction of graphene oxide can only partially remove the oxygen-containing groups.

Method used

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  • Preparation method of high-conductivity and high-elasticity three-dimensional graphene material
  • Preparation method of high-conductivity and high-elasticity three-dimensional graphene material

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Experimental program
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Effect test

Embodiment 1

[0053] Graphene oxide was synthesized by a modified Hummers method. Graphite powder (4.0 g, 325 mesh) and sodium nitrate (4.0 g) were added to concentrated sulfuric acid (192 mL), and stirred slowly in an ice bath for 20 minutes. Potassium permanganate (24.0 g) was then slowly added to keep the temperature of the suspension below 5° C. for 2 hours, and then the suspension was heated to 35° C. for two hours to form a thick slurry. Add deionized water (400mL) gradually afterwards, heat to 80 ℃ and keep warm for 20 minutes, then add 20 milliliters of hydrogen peroxide (30%), and finally add water to dilute the mixed solution to 1000 milliliters, leave it for a day, and finally put the product into a dialysis bag for dialysis to neutral;

[0054] Afterwards, the three-dimensional porous graphene material was prepared by hydrothermal reduction method, and 30 mL of graphene oxide solution (4 mg / mL) was ultrasonically treated for 1 hour (2 kW), sealed in a 50 mL tetrafluoroethylene a...

Embodiment 2

[0057] The preparation method in Example 2 is basically the same as that in Example 1, except that a small amount of water vapor (2 μg) is introduced before heating in a vacuum furnace with two temperature zones. The graphene oxide solution preparation method and reduction hydrothermal method are the same as in Example 1, and then the above-mentioned sample is placed in the low-temperature zone of the double-zone vacuum furnace, and the metal aluminum powder is placed in the high-temperature zone. Use a mechanical pump to evacuate to about 0.5Pa to remove the air in the furnace. Then a small amount of water vapor (2 μg) was introduced, and then the metal aluminum powder was heated to 800°C, the sample was heated to 200°C, and the heating was started at the same time, and the holding time was 4 hours, and finally the three-dimensional graphene material was obtained. The electrical conductivity of gained three-dimensional graphene material is 675.5S / m, and elastic modulus is 145...

Embodiment 3

[0059] The preparation method in Example 3 is basically the same as that in Example 2, except that a crosslinking agent glycolic acid is added to the graphene oxide solution at a concentration of 1 mg / ml. During the reaction, 30ml of a mixed solution containing glycolic acid (1mg / mL) and graphene oxide (4mg / mL) was stirred and sonicated for 1 hour (2kW) and sealed in a 50ml tetrafluoroethylene autoclave, then Put into 120 ℃ oven and keep for 12 hours, after cooling to room temperature, wash and soak the formed hydrogel with ethanol aqueous solution (20wt.%), then obtain three-dimensional porous graphene material by freeze-drying process, after the above-mentioned sample Put it in the low temperature zone of the double-zone vacuum furnace, and put the metal aluminum powder in the high temperature zone. Use a mechanical pump to evacuate to about 0.5Pa to remove the air in the furnace. After injecting a small amount of water vapor (2μg), heat the metal aluminum powder to 800°C, ...

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Abstract

The invention relates to a preparation method of a high-conductivity and high-elasticity three-dimensional graphene material. The preparation method comprises the following steps: (1) preparing a three-dimensional graphene material through a hydrothermal reduction method; and (2) respectively placing the metal aluminum powder and the three-dimensional graphene material in a low-temperature area and a high-temperature area of a double-area vacuum furnace, introducing a certain amount of water vapor, heating at the same time, setting the temperature of the low-temperature area to be 150-300 DEG C and the temperature of the high-temperature area to be 700-900 DEG C, and carrying out heat preservation for 2-6 hours to obtain the high-conductivity and high-elasticity three-dimensional graphene material.

Description

technical field [0001] The invention relates to a preparation method of a highly conductive and highly elastic three-dimensional graphene material, belonging to the field of three-dimensional graphene. Background technique [0002] Due to the excellent electronic and mechanical properties of graphene, the assembly of 2D graphene nanosheets into 3D structures has attracted extensive attention in recent years. The three-dimensional graphene structure combines the excellent intrinsic properties of graphene and the three-dimensional porous structure, providing graphene materials with excellent mechanical properties and fast electron transport. Macroscopic three-dimensional graphene materials have excellent mechanical and electrical properties, and have aroused widespread interest in the fields of electronics, catalytic devices, sensors, and adsorption materials. The development of three-dimensional graphene with ultra-low temperature, superelasticity, strong mechanical flexibili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/196C01B32/184
CPCC01B32/196C01B32/184C01B2204/20C01B2204/26C01B2204/22
Inventor 黄富强钱佳豪毕辉
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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