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Method for preparing large-size high-quality graphene with controllable number of layers

A high-quality, graphene technology, which is applied in the field of large-size, high-quality graphene preparation with a controllable number of layers, can solve the problems of reduced electrical conductivity and large graphene defects, and achieves controllable layers, simple processes, and high production efficiency. high rate effect

Inactive Publication Date: 2014-09-24
安徽百特新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is simple to operate and environmentally friendly, but the obtained graphene has large defects and greatly reduces the conductivity

Method used

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  • Method for preparing large-size high-quality graphene with controllable number of layers
  • Method for preparing large-size high-quality graphene with controllable number of layers
  • Method for preparing large-size high-quality graphene with controllable number of layers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put 1 g flake graphite (500 μm particle diameter, carbon content >95%), 5 g chromium trioxide and 0.6 g potassium permanganate into a 100 mL single-necked round bottom flask, then add 12 mL glacial acetic acid (99.5% ), stirred and reacted in a water bath at 45°C for 2 days, filtered, washed repeatedly with water and acetone to remove unreacted chromium trioxide, and dried in a vacuum oven at 65°C to obtain 5th order GICs, as figure 1 As shown in a, its Raman spectrum is shown as figure 2 shown. From figure 2 It can be seen that the I of GICs D / I G The value is very small, indicating that there are few defects in the sheet and the degree of oxidation is low.

[0035] Then, 0.1 g of 5th-order GICs was put into 20 mL of hydrogen peroxide (30%), and after reacting at room temperature for 2 days, it was found that the graphite was continuously expanding, filtered, and washed with water to obtain worm-like graphene aggregates. The morphology of the swelling was observe...

Embodiment 2

[0038] Put 1 g flake graphite (500 μm particle diameter, carbon content >95%) and 17 g chromium trioxide into a 100 mL double-necked round bottom flask, set up an exhaust gas absorption device, and then add 14 mL concentrated hydrochloric acid (38% ), stirred the reaction in a water bath at 45 °C, and absorbed the tail gas with sodium hydroxide. After 2 days, it was filtered, washed repeatedly with water and acetone to remove unreacted chromium trioxide, and dried in a vacuum oven at 65 °C to obtain the second-order GICs.

[0039] Then, 0.1 g of the second-order GICs was put into 20 mL of hydrogen peroxide (30%), reacted at room temperature for 2 days, filtered and washed with water to obtain worm-like graphene aggregates.

[0040] Finally, the worm-like graphene aggregates were placed in 100 mL NMP for 30 min in a water bath to obtain a black suspension, which was centrifuged at 12000 rpm for 10 min, the upper layer was discarded, and NMP was added, centrifuged at 12000 rpm f...

Embodiment 3

[0042] Put 1 g flake graphite (particle diameter 500 μm, carbon content >95%) and 3 g chromium trioxide into a 100 mL single-necked round bottom flask, then add 10 mL glacial acetic acid (99.5%), and reflux at 122 °C After 2 h, filter, wash repeatedly with water and acetone to remove unreacted chromium trioxide, and dry in a vacuum oven at 65 °C to obtain third-order GICs.

[0043] Then, 0.1 g of third-order GICs was put into 20 mL of hydrogen peroxide (30%), reacted at room temperature for 2 days, filtered, and washed with water to obtain worm-like graphene aggregates.

[0044] Finally, the worm-like graphene aggregates were placed in 100 mL NMP for 30 min in a water bath to obtain a black suspension, which was centrifuged at 12000 rpm for 10 min, the upper layer was discarded, and NMP was added, centrifuged at 12000 rpm for 10 min, and repeated After centrifugation for 3 times, add NMP to the lower layer, centrifuge at 500 rpm for 30 min, repeat centrifugation and collect th...

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Abstract

The invention discloses a method for preparing large-size high-quality graphene with controllable number of layers, wherein graphite powder or flake graphite is mainly adopted as a raw material. The method specifically comprises the steps of intercalating the graphite raw material by virtue of an intercalating agent to initially weaken the intercalation interaction force and obtain different orders of graphite intercalation compounds (GICs); soaking the GICs in an appropriate expander, and then under the case that an auxiliary agent is added or not, enabling the intercalation materials to be quickly reacted with the expander to release a gases to obtain highly expanded wormlike graphene aggregate and further to cause the distances among graphene lamellar layers to be increased; and after certain processing, peeling, and then repeatedly centrifuging and dispersing to obtain a graphene dispersion with different numbers of layers. According to the method disclosed by the invention, the intercalation-expansion-peeling process is involved, raw materials are cheap, the reaction process is simple and easily controlled, and the number of layers of graphene is precisely controlled; the obtained graphene lamellar layers have the advantages of few defects, large size, high conductivity, high yield and the like, the large-scale industrial production is easily implemented, and the problems of high cost, low productivity, poor quality, small size, uncontrollable number of layers and the like in an existing graphene preparation technology are solved.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and relates to a method for preparing large-size, high-quality graphene with a controllable number of layers, specifically a method of using oxidant and acid solution as intercalation agents to obtain graphite interlayers with different layers. compound, and then add chemical reagents such as oxalic acid or hydrogen peroxide to make it react violently with the interlayer substance to release gas, stretch the graphene sheet, and after mechanical treatment, graphite exfoliation can be achieved, and high-quality graphene with a controllable number of layers can be obtained Methods. Background technique [0002] In 2004, the Geim group of the University of Manchester in the United Kingdom used the "micromechanical force splitting method" for the first time to obtain a single-layer or thin-layer two-dimensional atomic crystal-graphene. This discovery shocked the scientific community. and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 卢红斌林珊董雷张佳佳杨超
Owner 安徽百特新材料科技有限公司
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