Method for preparing graphene nano-sheet based on crystalline flake graphite

A technology of graphene nanosheets and graphite flakes, which is applied in the field of graphene, can solve the problems of complex production process, low yield of graphene, and amorphization by mechanical ball milling of solid-state media, and achieve simple process, high oxidation degree, and control side effects. The effect of the reaction

Inactive Publication Date: 2018-02-23
郴州国盛新材科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, none of the above methods can be used to prepare defect-free high-quality graphene in large quantities.
For example, although the mechanical exfoliation method can theoretically produce defect-free high-quality graphene, the yield of the resulting graphene is very limited
Although the vapor deposition method can be used to prepare large-area graphene, its production process is complicated, the preparation conditions are harsh, the production cost is high, and the separation and transfer process of graphene film is very difficult, so this method still has great potential. limitation
[0003] The mechanical ball milling method is not only simple to operate, economical and applicable, but also easy to apply to large-scale industrial production. Therefore, it has also become a new process for the large-scale preparation of few-layer graphene nanosheets and their composite materials. However, by traditional solid phase The wet ball milling process developed by ball milling has a low yield of graphene, and solid medium mechanical ball milling easily leads to amorphization
The thickness of graphite flakes obtained by traditional shimmy high-energy ball milling is relatively thick, and due to the action of mechanical stress, it is difficult to preserve the integrity of the lamellar structure, and it is easy to form an edge carbon vacancy structure

Method used

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  • Method for preparing graphene nano-sheet based on crystalline flake graphite
  • Method for preparing graphene nano-sheet based on crystalline flake graphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The present embodiment provides a kind of preparation method that prepares graphene nanoplate based on flake graphite, comprises the following steps:

[0032] S1. Preparation of oxidized flake graphite: add flake graphite and sodium nitrate to concentrated sulfuric acid, and gradually add KMnO while keeping it below 20°C 4 , keep stirring at low temperature for 1h, then raise the temperature to 35°C and stir for 30min, then raise the temperature to 65°C, add hydrogen peroxide dropwise, keep for 40min, wash by repeated centrifugation and filtration, and then vacuum dry to obtain graphite oxide flakes;

[0033] S2. Pre-stripping: place the oxidized flake graphite obtained in step S1 in a heating furnace, raise the temperature from room temperature to 260-305°C, the heating rate is 9.0°C / min, and keep feeding Ar gas at 3000ml / min to obtain Expanded graphene nanosheets, the expanded graphene nanosheets have an expansion factor of 235 times and a specific surface area of ​​...

Embodiment 2

[0040] The present embodiment provides a kind of preparation method that prepares graphene nanoplate based on flake graphite, comprises the following steps:

[0041] S1. Preparation of oxidized flake graphite: add flake graphite and sodium nitrate to concentrated sulfuric acid, and gradually add KMnO while keeping it below 20°C 4 , kept stirring at low temperature for 2 hours, then raised the temperature to 40°C and stirred for 30 minutes, then raised the temperature to 80°C, added hydrogen peroxide dropwise, kept for 40 minutes, washed by repeated centrifugation and filtration, and then vacuum-dried to obtain graphite oxide flakes;

[0042] S2. Pre-stripping: place the oxidized flake graphite obtained in step S1 in a heating furnace, raise the temperature from room temperature to 260-305°C, the heating rate is 9.0°C / min, and keep flowing Ar gas at 3000ml / min, The expanded graphene nanosheets were obtained. The expanded graphene nanosheets had an expansion factor of 300 times...

Embodiment 3

[0050] This embodiment is basically the same as Embodiment 1, the difference is that in step S3, the ball milling medium GeO 2 , the graphene nanosheets prepared in this example have about 6 layers.

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Abstract

The invention relates to the technical field of graphene nano-sheets, and discloses a method for preparing a graphene nano-sheet based on crystalline flake graphite. According to the preparation method, crystalline flake graphite serving as a raw material is oxidized by adopting low temperature, medium temperature and high temperature three stages, so that the side reaction in the graphite oxidizing process can be effectively controlled, and the graphite oxidizability can be improved; the graphite oxide is pre-stripped at a low temperature, which has lower cost in comparison with that for high-temperature stripping at about 1000 DEG C, and is applicable to industrial application. The ball mill method assisted with discharge plasma is adopted, the preparation method is simple in process andcan be produced in a large scale, has relatively small damage to graphite lamella, few-layer graphene nano-sheet with relatively good crystallinity can be easily obtained, and a good reduction effectcan be achieved for graphite by adding a solid-state ball mill medium, and the prepared graphene nano-sheet has high quality and a multi-fold translucent yarn structure.

Description

technical field [0001] The present invention relates to the technical field of graphene, more specifically, to a method for preparing graphene nanosheets based on flake graphite. Background technique [0002] Graphene is a two-dimensional planar single-layer structure of carbon formed by sp2 hybridized carbon atoms bonded in the form of a hexagonal lattice, which is an allotrope of carbon. Graphene is the basic unit for constructing other dimensional carbon materials. When it changes in the way of wrapping, winding and stacking, it can form zero-dimensional fullerene, one-dimensional carbon nanotube and three-dimensional graphite respectively. Graphene has good electrical and optical properties, mechanical properties, thermal conductivity and extremely high charge carrier mobility, as well as excellent mechanical strength and flexibility. These properties of graphene make it attract a lot of attention and quickly become a research hotspot. Graphene and its derivatives trea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B2204/04
Inventor 李丽萍
Owner 郴州国盛新材科技有限公司
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