Preparation method of large-domain graphene single crystal

A graphene and single crystal technology, applied in the field of large-domain graphene single crystal preparation, can solve the problems of large wrinkle density, small domain size defect density distribution, and limit the application of graphene, so as to achieve the effect of improving quality

Active Publication Date: 2022-08-02
BEIJING GRAPHENE INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, due to the lack of stable growth process and reliable manufacturing equipment, most of the graphene films mass-produced by the traditional chemical vapor deposition method are polycrystalline films, with small domain size and wide defect density distribution, and surface roughness High, wrinkle density, and the quality of graphene products sold in the market vary, which greatly limits the application of graphene in high-end electronic devices and optoelectronics

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  • Preparation method of large-domain graphene single crystal
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  • Preparation method of large-domain graphene single crystal

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preparation example Construction

[0024] The application provides a method for preparing a large domain graphene single crystal, comprising the following steps:

[0025] 1) Anneal the sapphire / metal substrate in a small amount of oxidizing atmosphere;

[0026] 2) providing a growth gas in a manner of increasing the proportion of the growth gas in a gradient manner, and growing on the sapphire / metal substrate to obtain the large-domain graphene single crystal.

[0027] The preparation method of the large-domain graphene single crystal of the present invention adopts a chemical vapor deposition method and is carried out in a chemical vapor deposition device. The chemical vapor deposition equipment used can be various equipments known in the art, which will not be repeated here.

[0028] The method of the present application uses a sapphire / metal substrate as the growth substrate of the large-domain graphene single crystal, and the substrate can be prepared by a magnetron sputtering process. In the sapphire / met...

Embodiment 1

[0037] Example 1 Preparation of large domain graphene single crystal wafer on 4-inch Cu / sapphire single crystal substrate

[0038] Step (1): single crystal copper is prepared according to the method disclosed in the patent application with the application number of 201710522321.1, and a copper (111) single crystal with a thickness of 500 nm is obtained on a 4-inch sapphire single crystal substrate;

[0039] Step (2): The copper (111) single crystal thin film / sapphire was first subjected to a carrier gas flow rate of 4000 sccm Ar (wherein the oxygen content was 10 -5%, based on the total mass of argon), raised from room temperature to 1000°C for 1 hour, and annealed at 1000°C for 0.5h. After that, 20 sccm of diluted methane and 40 sccm of hydrogen were passed in, and the volume percentage of methane in the diluted carbon source gas was 0.1%. After 30 minutes of growth, the diluted methane was increased to 40sccm, and after 30 minutes of continued growth, the diluted methane wa...

Embodiment 2

[0040] Example 2 Preparation of large domain graphene single crystal wafer on 4-inch CuNi / sapphire single crystal substrate

[0041] Step (1): single crystal copper-nickel is prepared according to the method disclosed in the patent application with the application number of 201710522321.1, and a copper-nickel (111) single crystal with a thickness of 500 nm is obtained on a 4-inch sapphire single crystal substrate;

[0042] Step (2): The copper-nickel (111) single-crystal thin film / sapphire was first subjected to a carrier gas flow rate of 4000 sccm Ar (wherein the oxygen content was 10 -5 %, based on the total mass of argon), increased from room temperature to 1000 °C in 1 hour, and annealed at 1000 °C for 0.5h, passed 20sccm of diluted methane and 40sccm of hydrogen, the volume percentage of methane in the diluted carbon source gas was 0.1 %. After 3 minutes of growth, the diluted methane was increased to 40 sccm, and after 3 minutes of continued growth, the diluted methane ...

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Abstract

The invention provides a preparation method of a large-domain graphene single crystal. The preparation method comprises the following steps: 1) annealing a sapphire/metal substrate in a trace oxidizing atmosphere; and 2) providing growth gas according to a growth gas proportion gradient increasing mode, and growing on the sapphire/metal substrate to obtain the large-domain graphene single crystal. According to the method, the single-crystal graphene film is prepared on the single-crystal metal/sapphire wafer substrate by using an epitaxial and orientation consistent splicing method, and a certain degree of corners or defects occurring in the splicing process are overcome through a micro-aerobic passivation annealing and gradient gas supply mode, so that the prepared single-crystal graphene film is more perfect, and the performance of the single-crystal graphene film is improved. The quality of the obtained graphene film is greatly improved, the obtained graphene is in a single crystal form, the domain size of the obtained graphene single crystal is large, and the domain size is several times that of the graphene single crystal obtained by a conventional method.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular to a method for preparing a large domain graphene single crystal. Background technique [0002] Graphene has been widely studied due to its good physical and chemical properties, such as ultra-high carrier mobility, high light transmittance, and good mechanical properties, and has been widely used in transparent conductive films, photodetection, catalysis, biodetection, etc. and other fields have shown its potential practical value. [0003] Among the many preparation methods of graphene, the chemical vapor deposition method on the surface of copper foil has many advantages such as high quality of grown graphene and suitability for macro-scale preparation. Among the existing graphene film preparation methods, chemical vapor deposition is the preferred method for batch preparation of large-area high-quality graphene film materials. At present, due to the lack of stable growth proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/02C30B25/18
CPCC30B29/02C30B25/186
Inventor 阎睿唐际琳杜音王雅妮曹轶森彭海琳刘忠范
Owner BEIJING GRAPHENE INST
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