Preparation method of large-diameter graphene and large-diameter graphene

A graphene and large-scale technology, applied in the preparation of large-diameter graphene, large-diameter graphene, and graphene materials, can solve the problem of strong adsorption force between macromolecules and graphene, difficult to obtain large-diameter graphene, and difficult to achieve large-scale Preparation and other problems, to achieve the effect of easy recovery and reuse, easy to achieve industrial scale production, easy to industrialize large-scale popularization and application

Active Publication Date: 2020-04-17
昂星新型碳材料常州有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, it is mainly divided into the following categories: 1. Tape stripping method, using tape stripping repeatedly to obtain single-layer or few-layer graphene with a large sheet diameter, which is of high quality but difficult to achieve large-scale preparation; 2. Solution phase stripping method, in the solution phase In combination with ultrasound, high-speed shearing or ball milling to obtain graphene sheets from graphite layers, this method often requires the use of organic solvents and surfactants, and graphene sheets are easily broken during the preparation process, making it difficult to obtain large-diameter graphene; 3. The solid-phase ball milling method uses solid particles as a grinding aid, combined with ball milling, etc., to use friction under dry conditions to achieve the peeling of graphite to graphene, but this method also has a destructive effect on graphene sheets. The obtained graphene sheets are small in size and pollute the environment
4. Adhesive peeling method, which is very close to the "tape peeling method". Usually, a three-roller machine is used to repeatedly roll and peel graphite and adhesive, so that large-scale high-quality graphene can be obtained and large-scale production However, most of the adhesives used in this method are organic solvents, which are polluted, and the adsorption force between the polymer and graphene is strong, the removal cost is high in the later stage, and the polymer cannot be reused; or some adhesives need to be heated Under the circumstances, it can be repeatedly peeled off from graphite, and at high temperature, it may cause the coking of the adhesive, the solubility will decrease, and it will not be easy to remove when adsorbed on graphene. In addition, the regeneration cost of the adhesive is high, so it can be recycled bring obstacles

Method used

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  • Preparation method of large-diameter graphene and large-diameter graphene

Examples

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Effect test

Embodiment 1

[0075] A preparation method for large sheet diameter graphene, comprising the following steps:

[0076] (a) Prepare high-viscosity syrup: mix water, sucrose, glucose and fructose according to the ratio of water:sucrose:glucose:fructose=6:12:6:15 at room temperature 18-19°C, and use a Brookfield viscometer to test Its viscosity is 112000 centipoise;

[0077] (b) Mechanical exfoliation: 20g of the above-mentioned high-viscosity syrup is mixed with 0.5g and 100 mesh graphite powder, and the mixed material is transferred to a three-roll grinder, and the roll mill is 3h to obtain a mixture of graphene and syrup;

[0078] (c) Separation: add hot water at 70°C to the mixture of graphene and syrup obtained in step (b) to dissolve, centrifuge at 7000rpm for 10min, collect the supernatant of the first centrifugation, and then repeatedly wash and centrifuge the lower solid for 4 times to obtain large pieces diameter graphene;

[0079] (d) Recovery of syrup: The supernatant collected in...

Embodiment 2

[0083] A preparation method for large sheet diameter graphene, comprising the following steps:

[0084] (a) Prepare high-viscosity syrup: mix water, sucrose and fructose in the ratio of water: sucrose: fructose = 2:5:3 at a room temperature of 18-20°C, and measure its viscosity with a Brookfield viscometer to 245,000 centipoise ;

[0085] (b) Mechanical exfoliation: get 80g of the above-mentioned high-viscosity syrup and add 0.8g, 80-purpose expanded graphite, under an ice-water bath, adopt a high-speed disperser to carry out mechanical stirring for 3h to obtain a mixture of graphene and syrup;

[0086](c) Separation: add hot water at 70°C to the mixture of graphene and syrup obtained in step (b) to dissolve, centrifuge at 7000rpm for 10min, collect the supernatant of the first centrifugation, and then repeatedly wash and centrifuge the lower solid for 4 times to obtain large pieces diameter graphene;

[0087] (d) Recovery of syrup: The supernatant collected in step (c) is s...

Embodiment 3

[0090] A kind of preparation method of large diameter graphene, and the difference of embodiment 2 is:

[0091] (b) mechanical exfoliation: get 100g high-viscosity syrup and add 2g, 80 purpose expanded graphite, under ice-water bath, adopt high-speed disperser to carry out mechanical stirring for 5h, obtain the mixture of graphene and syrup;

[0092] All the other are with embodiment 2.

[0093] Take a small amount of centrifuged lower layer solid, add 25mL DMF to sonicate for 20min, make slices on glass slides, and observe the effect under a microscope. Figure 4 , the actual length and width dimensions corresponding to the picture are 141 μm×106 μm.

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Abstract

The invention belongs to the technical field of nanometer materials, relates to a graphene material, and particularly relates to a preparation method of a large sheet diameter graphene and the large sheet diameter graphene. The provided preparation method of the large sheet diameter graphene takes graphite as the raw material and high-viscosity syrup as a peeling auxiliary, the large sheet diameter graphene is prepared by means of mechanical peeling; wherein the viscosity range of the syrup is 5*10<4> to 1.5*10<6> centipoise. Meanwhile, the syrup is regenerated and recycled through the simplereduced pressure distillation after the separation, the process is simple, the condition is mild, the cost is low, the preparation method is efficient and environmentally friendly, and the prepared graphene material has the advantages of large sheet diameter and high electrical conductivity.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials and relates to graphene materials, in particular to a preparation method of large-diameter graphene and large-diameter graphene. Background technique [0002] Graphene is a two-dimensional carbon material with excellent electrical, thermal, and mechanical properties. It has attracted extensive attention in many fields such as energy, electronic materials, biomedicine, and environmental protection. Necessary conditions for its application development. Existing graphene preparation techniques include chemical reduction of graphene oxide, vapor deposition, crystal epitaxial growth, mechanical exfoliation, etc., wherein chemical reduction of graphene oxide and mechanical exfoliation are methods that are easy to achieve large-scale production, but The chemical reduction method will inevitably produce pollution, and there are certain safety issues, and the prepared graphene has many defects...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
Inventor 陈武峰赖斌张晓平
Owner 昂星新型碳材料常州有限公司
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