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A kind of preparation method of monolayer graphene

A single-layer graphene and vacuum chamber technology, applied in the direction of single-layer graphene, graphene, chemical instruments and methods, etc., can solve the problems of difficulty in effectively controlling the number of graphene layers, uneven number of layers, small size of graphene, etc. , to achieve the effect of simple and controllable preparation method, avoiding uneven thickness, and realizing controllable operation

Active Publication Date: 2020-04-07
INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, there are still many problems in these methods. For example, in the process of thermal decomposition, it is easy to produce island-shaped nucleation growth, the number of layers is uneven, and the size of graphene is small. More importantly, the graphene produced by these methods The number of layers cannot be controlled
Chinese patent CN102936009A discloses a method for preparing a low-layer graphene film by thermal decomposition. In this method, a silicon carbide substrate with a silicon surface is selected to be placed on a graphite base with a tantalum carbide coating, and argon gas is introduced and Control heating and cooling to start the carbonization process, so as to achieve stable and controllable effective carbonization time. Although this method realizes the preparation of graphene film with low number of layers, it is difficult to effectively control the number of graphene layers obtained by this method, and the generated graphite Graphene films occasionally have discontinuous nucleation defects, which cannot meet the market demand for large-area high-quality single-layer graphene.

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  • A kind of preparation method of monolayer graphene
  • A kind of preparation method of monolayer graphene
  • A kind of preparation method of monolayer graphene

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preparation example Construction

[0027] The invention provides a kind of preparation method of monolayer graphene, comprises the steps:

[0028] (1) Take the SiC substrate and clean and dry it sequentially, then put it into the crucible;

[0029] (2) Place the crucible in a vacuum chamber, fill it with inert gas under vacuum conditions until the pressure in the vacuum chamber is 300-600 Torr, close the vacuum chamber, and then inductively heat the crucible to raise the temperature of the SiC substrate to the pyrolysis temperature for heat preservation;

[0030] (3) Adjust the air pressure to 5-30 Torr, and control the inert gas in the vacuum chamber to maintain the dynamic balance of the air pressure, so that the SiC substrate can be pyrolyzed;

[0031] (4) After the pyrolysis is completed, adjust the air pressure in the vacuum chamber to 450-550 Torr, then stop the induction heating, let the crucible drop to room temperature naturally, feed inert gas into the vacuum chamber to normal pressure, take out the s...

Embodiment 1

[0041] A preparation method of monolayer graphene, specifically comprises the steps:

[0042] (1) Take a commercially available research-grade 4H-SiC substrate with a diameter of 4 inches and a thickness of 200 μm, clean and dry in sequence, and put it into a graphite crucible with the Si side facing upward;

[0043] (2) Place the crucible in a vacuum chamber, and first evacuate to a vacuum degree of 5×10 -7 Torr, then pass in argon to keep the pressure in the vacuum chamber at 500Torr; close the vacuum chamber, then heat the crucible by induction to raise the temperature of the SiC substrate, and keep the temperature stable after heating to 1800°C, and keep it warm for 3.5h;

[0044] (3) Turn on the mechanical pump to extract the vacuum while continuously feeding argon gas into the vacuum chamber. The flow rate of argon gas is 50 sccm, the air pressure in the vacuum chamber is stable at 5 Torr, and the air pressure dynamic balance is achieved. Bottom pyrolysis;

[0045] (4)...

Embodiment 2

[0049] A preparation method of monolayer graphene, specifically comprises the steps:

[0050] (1) Take a commercially available research-grade 4H-SiC substrate with a diameter of 4 inches and a thickness of 200 μm, clean and dry in sequence, and put it into a graphite crucible with the C side facing upward;

[0051] (2) Place the crucible in a vacuum chamber, and first evacuate to a vacuum degree of 5×10 -7 Torr, then pass in argon gas to keep the pressure in the vacuum chamber at 500 Torr; close the vacuum chamber, then heat the crucible by induction to raise the temperature of the SiC substrate, and keep the temperature stable after heating to 2000°C, and keep it warm for 3 hours;

[0052] (3) Turn on the mechanical pump to extract the vacuum while continuously feeding argon gas into the vacuum chamber. The flow rate of argon gas is 200 sccm, the air pressure in the vacuum chamber is stable at 15 Torr, and the dynamic balance of air pressure is achieved. Substrate pyrolysis...

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Abstract

The invention provides a preparation method of monolayer graphene. The monolayer graphene is prepared through performing heating for pyrolysis on an SiC substrate in air pressure dynamic equilibrium environment filled with inert gas. The preparation method specifically comprises the following steps: taking the SiC substrate, performing pretreatment, and putting the pretreated SiC substrate in a crucible; placing the crucible in a vacuum chamber, performing vacuumizing, charging the inert gas, performing induction heating on the crucible so as to urge the SiC substrate to raise the temperatureto pyrolysis temperature, and preserving the temperature; adjusting air pressure, controlling the inert gas in the vacuum chamber, maintaining air pressure to be in dynamic equilibrium, and enabling the SiC substrate to be subjected to pyrolysis; and after the pyrolysis is completed, reducing the temperature to a room temperature, recovering the pressure to the normal pressure, and taking out themonolayer graphene. The preparation method provided by the invention is simple and controllable, the production efficiency is improved, and batch production can be performed hopefully. Through the adoption of the method, large-sized monolayer graphene of 2-4 inches can be prepared, the layer number of the monolayer graphene can be controllable, the area is large, few lattice defects exist, and themarket demands for high-quality monolayer graphene can be met.

Description

technical field [0001] The invention belongs to the technical field of preparation of graphene functional materials, and in particular relates to a preparation method of single-layer graphene. Background technique [0002] Graphene is a sp 2 A two-dimensional atomic crystal with a hexagonal honeycomb structure closely packed with carbon atoms. As an ideal two-dimensional atomic crystal, graphene has ultra-high electrical conductivity, thermal conductivity, strength and huge theoretical specific surface area. Its structure Extremely stable, it is the strongest and hardest crystal structure among known materials. Among them, the thickness of single-layer graphene is only 0.35nm, which is the thinnest material known so far. [0003] Due to the intrinsic characteristics of graphene, it shows great application potential in the fields of semiconductor, photovoltaic, energy, aerospace, national defense and military industry: graphene material has a large specific surface area, pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01B32/184C01B2204/02C01B2204/32C01P2002/01C01P2002/82
Inventor 张贺古宏伟丁发柱李辉屈飞
Owner INST OF ELECTRICAL ENG CHINESE ACAD OF SCI