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Thin-layer low-defect micro-nano graphene and preparation method thereof

A graphene, micro-nano technology, applied in the field of graphene, can solve the problems of difficult industrial production and application, high cost, high defects, etc., and achieve the effect of being suitable for industrial promotion and application, simple method and low defect degree

Active Publication Date: 2022-02-22
HAIKE GRP RES INST OF INNOVATION & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, although graphene has excellent performance, in practical applications, graphene still has many problems and restrictive factors. As far as its preparation method is concerned, the graphene prepared by the existing physical exfoliation method is mostly in water system and oil. It is prepared under the system, and there is a graphene drying step, which leads to serious graphene folding back, graphene characteristics are not significant, and nano-scale graphene with a smaller thickness cannot be obtained; while graphene prepared by redox has more surface functional groups , and the defect is high
Limit the scope of application of graphene
The laboratory-level CVD preparation process is too cumbersome, the conditions are harsh, the output rate is low, the cost is high, and the production efficiency is affected. It is not suitable for mass production, and it is difficult to realize large-scale industrial production and popularization and application.

Method used

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  • Thin-layer low-defect micro-nano graphene and preparation method thereof
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  • Thin-layer low-defect micro-nano graphene and preparation method thereof

Examples

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preparation example Construction

[0069] In principle, the present invention has no special restrictions on the preparation route of the graphene, and those skilled in the art can select and adjust according to actual production conditions, product requirements and quality requirements. The present invention further improves the thinness of graphene and reduces surface functional groups. and degree of defect, ensuring its specific structure, and finally improving the quality of graphene, which is preferably obtained from graphite through high-pressure exfoliation, weak edge oxidation and intercalation.

[0070] The invention provides a kind of preparation method of micro-nano-scale graphene, it is characterized in that, comprises the following steps:

[0071] 1) After graphite is mixed with a solvent, a graphite premix is ​​obtained;

[0072] 2) After the graphite premix obtained in the above steps is stripped off, an intermediate product is obtained;

[0073] 3) After the intermediate product obtained in the...

Embodiment 1

[0115] Mix 10g of expanded graphite and 990g of NMP evenly, and carry out full solid-liquid mixing in a vacuum defoaming stirring tank for 1 hour. Graphene: concentrated sulfuric acid: potassium permanganate carries out weak oxidation reaction by the mass ratio of 1:100:1, after the graphene after reaction is filtered, according to graphene: potassium sodium tartrate tetrahydrate: deionized water 1:100: The mass ratio of 1 was used for intercalation and stripping experiments. After reacting in a constant temperature water bath at 80°C for 4 hours, it was treated with ultrasonic stirring for 30 minutes to obtain a nano-graphene mixed solution, which was centrifuged at 1000r / min to obtain an upper-layer nano-graphene solution, and then filtered to obtain a nano-graphene solution. Graphene powder.

[0116] The micro-nano-scale graphene prepared in Example 1 of the present invention was characterized.

[0117] see figure 1 , figure 1 It is an AFM atomic force microscope sheet r...

Embodiment 2

[0122] Mix 10g of expanded graphite and 990g of NMP evenly, and carry out solid-liquid mixing in a vacuum defoaming stirring tank for 1 hour. The premixed material is crushed and peeled off 5 times by a high-pressure homogenizer under a pressure of 200MPa to prepare a submicron-sized graphene microflake, graphite Graphene: Concentrated sulfuric acid: Potassium permanganate is subjected to a weak oxidation reaction according to the mass ratio of 1:100:1, and the graphene after the reaction is filtered, according to the ratio of graphene: sodium sulfate decahydrate: deionized water 1:100:1 The mass ratio was used for intercalation and stripping experiments. After reacting in a constant temperature water bath at 80°C for 4 hours, it was treated with ultrasonic stirring for 30 minutes to obtain a nano-graphene mixture, which was centrifuged at 1000r / min to obtain an upper-layer nano-graphene solution, and then filtered to obtain nano-graphene. Powder.

[0123] The micro-nano-scale...

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Abstract

The invention provides micro-nano graphene. The sheet layer edge of the graphene is graphene oxide; and other parts, except the edge position, of a graphene sheet layer are graphene. According to the preparation method, the micro-nano graphene with a specific structure is obtained, and the graphene has a micron-scale large sheet diameter and a nano-scale thinness, and has the same structure and characteristics as graphene oxide at the edge of the sheet layer. The micro-nano graphene provided by the invention has a graphene structure with less than 5 layers of lamellas, has lower surface functional groups and defect degree and higher graphene quality, and is thin-layer low-defect graphene. According to the preparation method provided by the invention, preparation is carried out through mechanical stripping, weak oxidation and chemical shallow insertion technologies; and the method is simple in process, low in cost and more suitable for industrial popularization and application.

Description

technical field [0001] The invention belongs to the technical field of graphene, and relates to a micro-nano-scale graphene and a preparation method thereof, in particular to a thin-layer low-defect micro-nano-scale graphene and a preparation method thereof. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a carbon atom with sp 2 The hybrid orbitals form a hexagonal planar film with a honeycomb lattice, with sp 2 The carbon six-membered ring two-dimensional crystal structure formed by hybridization is the basic unit for constructing other dimensional carbon materials. Its basic structural unit is the most stable benzene six-membered ring in organic materials, with a theoretical thickness of only 0.335nm and a two-dimensional material with a thickness of only one carbon atom, which is the thinnest two-dimensional material among known materials discovered so far. Since Geim et al first prepared grap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/19C01B32/198
CPCC01B32/184C01B32/19C01B32/198C01B2204/32C01B2204/04Y02P20/54
Inventor 吴炳辉杨亚东赵兴涛
Owner HAIKE GRP RES INST OF INNOVATION & TECH
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