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Graphene solution and preparation method thereof

A single-layer flake, graphite technology, applied in the field of graphite single-layer flake solution and its preparation, can solve the problems of limiting the modification and application of graphite single-layer flake

Inactive Publication Date: 2012-05-23
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the defect that the graphite monolayer solution prepared by the prior art is easy to stack and aggregate, thereby limiting the further modification and application of the graphite monolayer, and to provide a high-concentration and no need to add surfactant Modified graphite monolayer solution and preparation method thereof

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  • Graphene solution and preparation method thereof
  • Graphene solution and preparation method thereof
  • Graphene solution and preparation method thereof

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preparation example Construction

[0021] The method for preparing the graphite single-layer sheet solution of the present invention comprises heating the graphite single-layer sheet oxide organic phase solution with a concentration of 0.1-1mg / mL at 90-200°C for 2-12 hours under airtight conditions, and carrying out Heat treatment; preferably heating at 100-180° C. for 2-10 hours for heat treatment.

[0022] Preferably, in order to disperse the graphite single-layer oxide organic phase solution before the heat treatment more uniformly, so that the graphite single-layer oxide solution obtained after the heat treatment is more stable, the graphite single-layer oxide organic phase solution can be carried out in advance Ultrasonic treatment, the method of the ultrasonic treatment can adopt the conventional ultrasonic treatment method, which will not be described in detail here.

[0023] Preferably, the method of the present invention further includes centrifuging the heat-treated product to obtain a graphite single...

Embodiment 1

[0042] Prepare a deionized aqueous solution of graphite monolayer oxide.

[0043] At 20°C, 2.0 g of fineness of 325 mesh flake graphite and 1.5 g of sodium nitrate were added to 80 mL of concentrated sulfuric acid (98% by weight), and the resulting mixture was placed in a 500 mL beaker and cooled with an ice-water bath for 30 min. To a temperature of 8°C, a suspension was obtained.

[0044] At 5°C, at a stirring speed of 700r / min (the size of the stirring bar: 6cm), add 9.0g of potassium permanganate to the above suspension (adding once every 15 minutes, adding 1.5g each time), Then the ice-water bath was removed and kept for 120 hours, and 150 mL of deionized water was added (50 mL every 5 minutes), and half an hour later, 250 mL of 3 wt% hydrogen peroxide was added to obtain a bright yellow solution. Centrifugal washing with deionized water until there is no sulfate ion in the bright yellow solution, and then the solution is centrifuged (2560 × g, 3000rpm) to obtain a 6mg / m...

Embodiment 2

[0046] A DMF solution of graphite monolayer oxide was prepared.

[0047] Get the deionized aqueous solution of the graphite monolayer oxide in the preliminary example 1, centrifuge for 30 minutes (12400 × g, 11000rpm), remove the supernatant, then add N, N-dimethylformamide (DMF, Beijing Chemical Industry Co., Ltd. Factory, Beihua reagent) to the volume of the deionized aqueous solution of the initial graphite monolayer oxide, redisperse, centrifuge again for 30 minutes (12400 × g, 11000rpm), remove the supernatant, and then redisperse with DMF, repeat the above Operate 5 times to obtain the DMF solution of graphite single-layer oxide, the concentration of graphite single-layer oxide is 4mg / mL, and the ratio of the carbon number of graphite single-layer oxide to the number of oxygen atoms is C / O=2 .

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Abstract

The invention discloses a graphene solution, comprising an organic solvent and graphene, wherein, the organic solvent is an amide solvent and / or an alkanone solvent, and the concentration of the graphene is 0.06-0.6 mg / mL. The preparation method comprises the following steps: under enclosed conditions, heating a graphene organic phase solution having a concentration of 0.1-1 mg / mL for 2-12 h at a temperature of 90-200 DEG C, and carrying out heat treatment. The concentration of graphene in the graphene solution is larger than 0.06 mg / mL. Compared with graphene solutions obtained without adding a stabilizing agent in the prior art, the concentration of graphene in the graphene solution disclosed herein is greatly increased. According to the invention, by using the amide and / or alkanone solvent as the organic solvent and the introduction of reducing agent or stabilizing agent molecules is not needed additionally in the process of reducing the organic phase solution of graphene oxides. The invention has a wide application prospect in the field of graphene materials and devices.

Description

technical field [0001] The invention relates to a graphite monolayer sheet solution and a preparation method thereof. Background technique [0002] Graphene, commonly known as graphene, has attracted the attention of researchers in recent years due to its advantages in electrical, thermal and mechanical properties. Materials and devices based on graphite single-layer sheets have broad application prospects in many fields such as energy storage materials, biosensing, gas adsorption and catalytic materials. As the building block of these materials and devices, whether graphite single-layer sheets can be prepared with high quality and high yield has become the bottleneck and cornerstone for the real production and application of these materials and devices (Dreyer, D.; Park, S. .; Bielawski, C. Chem. Soc. Rev. 2010, 39, 228-240). [0003] At present, the preparation methods of graphite single-layer sheets can be mainly divided into five types: chemical vapor deposition method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/20
Inventor 韩宝航周鼎承倩怡
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA