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Preparation method of large-area few-layer graphene and dispersion solution thereof

A technology of few-layer graphene and dispersion liquid, which is applied in the field of graphene material preparation, can solve the problems of complex process, environmental pollution, harsh conditions, etc., and achieve the effect of simple preparation process, wide application range and high peeling degree

Inactive Publication Date: 2015-04-22
QINGDAO UNIV OF SCI & TECH
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  • Description
  • Claims
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Problems solved by technology

[0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, chemical vapor deposition method, epitaxial growth method and chemical redox method, etc. These methods have their advantages and disadvantages: mechanical exfoliation method is not suitable for large Large-scale industrial production of graphene; chemical vapor deposition method and epitaxial growth method have disadvantages such as complicated process, harsh conditions, low yield and high cost, which limit their large-scale industrial production and application of graphene; although redox method is currently the Large-scale preparation of graphene is a relatively common method, but the traditional Hummer method has high energy consumption and is easy to pollute the environment, and the obtained graphene has many defects and is prone to aggregation, and the formed graphene dispersion has poor stability and the size of graphene smaller

Method used

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  • Preparation method of large-area few-layer graphene and dispersion solution thereof
  • Preparation method of large-area few-layer graphene and dispersion solution thereof
  • Preparation method of large-area few-layer graphene and dispersion solution thereof

Examples

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Embodiment 1

[0022] When the present embodiment prepares the large-area few-layer graphene dispersion liquid, it specifically includes the following steps:

[0023] (1) get 5g purity and be that 99% sheet diameter size is the mixed acid that the natural flake graphite 5g of 150 μm is formed with 30ml concentrated nitric acid and the vitriol oil mixes evenly, wherein the volume of concentrated nitric acid is 10ml, and the volume of vitriol oil is 20ml; Then add 10ml Hydrogen peroxide, stirred and reacted at 35 degrees for 1 hour, filtered, washed with water to pH = 7, dried at 60 degrees Celsius for 10 hours to obtain layered graphite;

[0024] (2) Add 2 g of delaminated graphite to aqueous hydrochloric acid solution, adjust the pH value to 1, filter and wash with water after soaking for 5 minutes, and dry at 60 degrees Celsius for 12 hours to obtain acidified delaminated graphite;

[0025] (3) Take 1 g of acidified delaminated graphite and add it to 200 ml of ethanol, add 1 g of sodium dod...

Embodiment 2

[0033] The other steps of this embodiment are the same as those in Example 1, only water is used as solvent in the preparation process of step (3) graphene dispersion liquid, and the graphene aqueous solution obtained is as follows figure 1 As shown in b, the sample is dispersed evenly, the concentration can reach 2mg / ml, and it can keep for two weeks without sedimentation.

Embodiment 3

[0035] The other steps of this embodiment are the same as those in Example 1, only use tetrahydrofuran as solvent in the preparation process of step (3) graphene dispersion liquid, the tetrahydrofuran dispersion liquid of the obtained graphene is as follows figure 1 As shown in c, the sample dispersion is very uniform, the concentration can reach 2mg / ml, and it will not settle for one month.

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Abstract

The invention belongs to the technical field of preparation of graphene materials, and particularly relates to a preparation method of large-area few-layer graphene and a dispersion solution thereof. The preparation method comprises the following steps: uniformly mixing natural crystalline flake graphite and mixed acid composed of concentrated nitric acid and concentrated sulfuric acid in a reactor, adding oxydol, reacting while stirring, then filtering, washing with water, and drying to obtain layered graphite; immersing the layered graphite in a volatile acid water solution, and sequentially filtering, washing with water and drying to obtain acidified layered graphite; and adding the acidified layered graphite into solvent containing surfactant, and performing ultrasonic exfoliation to obtain the graphene dispersion solution. The preparation method is simple in preparation process and convenient to operate; and the prepared graphene and graphene dispersion solution are superior in quality. The preparation method is wide in application range, environment-friendly, energy-saving and suitable for large-scale production.

Description

Technical field: [0001] The invention belongs to the technical field of graphene material preparation, in particular to a method for preparing large-area few-layer graphene and its dispersion. Background technique: [0002] Graphene is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. It has very excellent properties, for example, its specific surface area is as high as 2630m 2 .g -1 , sign mobility up to 200000cm 2 .v -1 .s -1 , Young's modulus up to 1.0TPa, thermal conductivity constant of 5000W.m -1 .K -1 , the optical transmittance is as high as 97.7%, and these properties of graphene make this new material attract widespread attention. [0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, chemical vapor deposition method, epitaxial growth method and chemical redox method, etc. These methods hav...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 刘睿宗成中王春芙
Owner QINGDAO UNIV OF SCI & TECH
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