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Graphene aerogel microsphere and preparation method thereof

A technology of graphene airgel and graphene hydrogel, applied in graphene, chemical instruments and methods, inorganic chemistry, etc. The materials are difficult to prepare and other problems, and the effects of shortening the preparation cycle and cost, simple equipment operation and easy filling are achieved.

Active Publication Date: 2017-12-05
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the preparation of larger-sized graphene airgel is more complicated in process, and it is difficult to prepare special-shaped airgel materials, and it is not easy to compound and blend bulk airgel with other materials.

Method used

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  • Graphene aerogel microsphere and preparation method thereof
  • Graphene aerogel microsphere and preparation method thereof
  • Graphene aerogel microsphere and preparation method thereof

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preparation example Construction

[0030] Another aspect of the embodiments of the present invention also provides a method for preparing the graphene airgel microspheres, comprising the steps of:

[0031] (1) Provide graphene oxide aqueous dispersion;

[0032] (2) Uniformly mixing the graphene oxide aqueous dispersion with a reducing agent to form a mixed solution;

[0033] (3) spraying the mixed liquid into monodisperse micro-droplets, and receiving the micro-droplets with a powder aggregated from hydrophobic particles to obtain liquid marbles of graphene oxide aqueous dispersion;

[0034] (4) making the liquid marbles gel to obtain graphene hydrogel microspheres;

[0035] (5) removing the hydrophobic particles attached to the surface of the graphene hydrogel microspheres, and then performing solvent replacement and drying to obtain graphene airgel microspheres.

[0036] In some typical implementation cases, the concentration of the graphene oxide aqueous dispersion is 1-20 mg / ml; and / or, the graphene oxide...

Embodiment 1

[0051] (a) Preparation of graphene oxide micro-droplets: Measure the graphene oxide aqueous dispersion with a concentration of 5 mg / ml, add ascorbic acid according to the mass ratio of ascorbic acid and graphene oxide at a ratio of 5:1, and keep stirring to make it Dissolve completely, use the microarray spotter as the device for preparing micro-droplets, and spray the micro-droplets into the hydrophobic particle substrate, and the diameter of the sprayed micro-droplets is 750um;

[0052] (b) Preparation of graphene airgel microspheres: the hydrophobic particles used were hydrophobic fumed silica, and the gel was left to stand at 20°C for 24 hours. The graphene hydrogel microspheres are washed with ethanol, and then hydrofluoric acid is used to wash away the residual hydrophobic fumed silica, and then the solvent is replaced by ethanol, and finally the graphene airgel microspheres are obtained by supercritical drying.

[0053] The structure and performance characterization of th...

Embodiment 2

[0055] (a) Preparation of graphene oxide micro-droplets: Measure the graphene oxide aqueous dispersion with a concentration of 15 mg / ml, add ascorbic acid according to the mass ratio of ascorbic acid and graphene oxide at a ratio of 5:1, and keep stirring to make it Dissolve completely, use the microarray spotter as a device for preparing micro-droplets, and spray the micro-droplets into the hydrophobic particle substrate, and the diameter of the sprayed micro-droplets is 1mm;

[0056] (b) Preparation of graphene airgel microspheres: the hydrophobic particles used are hydrophobic silica airgel, and the gel was left to stand at 25°C for 24 hours. The graphene hydrogel microspheres are washed with ethanol, and then hydrofluoric acid is used to wash away the residual hydrophobic silica airgel, and then the solvent is replaced by ethanol, and finally the graphene airgel microspheres are obtained by supercritical drying.

[0057] The structure and performance characterization of th...

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Abstract

The invention discloses a graphene aerogel microsphere and a preparation method thereof. The graphene aerogel microsphere contains a porous structure formed by aggregation of graphene. Aperture of pores contained in the porous structure is 1-500 nm, specific surface area of the graphene aerogel microsphere is 100-1000 m<2> / g, bulk density is less than 300 mg / cm<3>, and specific capacitance is 30-500 F / g. The preparation method comprises the following steps: providing a graphene oxide aqueous dispersion; mixing the graphene oxide aqueous dispersion and a reducing agent to form mixed liquor; spraying the mixed liquor to form monodispersed micro-droplets, carrying the micro-droplets by powder formed by aggregation of hydrophobic particles to obtain liquid marbles of the graphene oxide aqueous dispersion; turning the liquid marbles into gel to obtain graphene aerogel microsphere; and removing hydrophobic particles, and displacing through a solvent and drying to obtain the graphene aerogel microsphere. The method of the invention is simple. The prepared graphene aerogel microsphere has uniform and controllable size, has excellent performance, can realize continuous production, and has a huge application prospect.

Description

technical field [0001] The invention relates to a graphene airgel, in particular to a graphene airgel microsphere and a preparation method thereof, belonging to the technical field of nanoporous materials. Background technique [0002] The generation of aerogel originated in the 1930s, by California Pacific University chemist Steven. S. A substance that Kistler inadvertently invented, known colloquially as "frozen smoke," is made by extracting water from silica gel and replacing the water with a gas such as carbon dioxide. After more than 80 years of development, airgel materials have been gradually commercialized and have important applications in many fields. [0003] Graphene, as a new type of nanomaterial with excellent performance, has flourished in just ten years of development, and has made important progress and applications in various research fields. Graphene airgel uses graphene oxide as a precursor. After adding an appropriate reducing agent, the gel is left t...

Claims

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Application Information

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IPC IPC(8): C01B32/182C01B32/184
CPCC01B2204/22C01B2204/32C01P2004/03C01P2006/10
Inventor 张学同王叙春
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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