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Graphene single crystal and its rapid growth method

A graphene and single crystal technology, applied in the field of materials, can solve the problems of reducing graphene nucleation density, energy consumption and gas consumption, and slow growth rate of graphene film

Active Publication Date: 2018-02-23
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional method of preparing large single-crystal graphene films usually uses copper foil as the catalyst and material growth substrate at high temperature, and uses extremely low carbon source supply and a large amount of reducing gas to reduce the nucleation density of graphene, and then obtain large single-crystal graphene films. Graphene film composed of single crystal graphene, but due to the limitation of carbon source supply in this method, the growth rate of graphene film is extremely slow, and the long-term high-temperature growth brings a lot of energy consumption and gas consumption

Method used

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  • Graphene single crystal and its rapid growth method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Example 1. Rapid preparation of large single crystal graphene

[0081] 1) The copper foil (produced by Alfa Aesar, with a purity of 99.8% and a thickness of 25 μm) was placed in a phosphoric acid ethylene glycol solution for electrochemical polishing. The phosphoric acid concentration was 85%, and the volume ratio of phosphoric acid and ethylene glycol was 3:1. The current density is maintained at 30A / m 2 -100A / m 2 In between, the polishing time is about 30min. The polished copper foil was rinsed with deionized water and blown dry with nitrogen.

[0082] 2) The above-mentioned polished copper foil is placed in a sleeve with magnetic force control, and the sleeve is placed in a large quartz tube of a tube furnace, heated to an annealing temperature of 1020° C. in an argon gas of 500 sccm, and the system pressure is 480Pa.

[0083] 3) After the temperature was raised to 1020° C., 100 sccm of hydrogen was introduced, and the system pressure was 100 Pa, and annealed in ...

Embodiment 2、 3

[0093] Example 2. Three-stage accelerated growth of large single-crystal graphene

[0094] Step 1) to step 6) are the same as step 1) to step 6) of Example 1;

[0095] 7) Keep the system at 1020°C, turn off the argon gas, feed 60 sccm of hydrogen and 0.2 sccm of methane into the system, and keep for 15 minutes for secondary growth. Under this condition, graphene can grow along the graphene island in step 5). Epitaxial growth.

[0096] 8) Cut off methane and hydrogen successively, feed 100sccm of mixture gas composed of argon and oxygen into the system, keep 20s for three passivation, rely on a small amount of oxygen in argon to passivate the copper foil again, reduce active sites, reduce Nucleation density.

[0097]9) Keep the system at 1020°C, turn off the argon gas, feed 20 sccm of hydrogen and 0.2 sccm of methane into the system, keep for 15 min for three growths, and then use a magnet to drag the sleeve with copper foil from the high temperature zone of the tube furnace....

Embodiment 3

[0103] Embodiment 3, prepare the thin film of large single crystal graphene splicing

[0104] Step 1) to step 6) are the same as step 1) to step 6) of Example 1;

[0105] 7) Keep the system at 1020°C, turn off the argon gas, and feed 60 sccm of hydrogen and 0.2 sccm of methane into the system for secondary growth. Under this condition, graphene can be epitaxially grown along the graphene island in step 5). After growing for 200min, use a magnet to pull the sleeve loaded with copper foil out of the high temperature area, quickly reduce the temperature of the sample to room temperature, and end the growth of the sample. Graphene film.

[0106] The grown copper foil sample was taken out, and a 4% mass fraction of PMMA ethyl lactate solution was suspended on the surface of the sample at a speed of 2000 rpm for 1 min; the sample was dried on a hot stage at 170 °C; 90W air was used. Plasma etched the reverse side of the sample for 5 min;

[0107] A ferric chloride solution with a...

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Abstract

The invention discloses a graphene single crystal and a rapid growth method thereof. The rapid growth method comprises carrying out primary passivation on annealed copper foil, orderly carrying out primary growth, secondary passivation and secondary growth at a constant temperature, and carrying out cooling to a room temperature so that crystal growth is stopped and the graphene single crystals are deposited on the copper foil, wherein in primary growth and secondary growth, growth gas comprises reduction gas and carbon source gas, and in secondary growth, the partial pressure of the carbon source gas in the growth gas is higher than that of the carbon source gas in the primary growth. The rapid growth method has simple processes and can be industrialized. The graphene single crystal has single crystal domain area size in a subcentimeter level and high single crystal quality and can be used in electronics.

Description

technical field [0001] The invention belongs to the field of materials, and relates to a graphene single crystal and a rapid growth method thereof. Background technique [0002] Graphene is a kind of carbon atom through sp 2 Monolayer or few-layer two-dimensional crystalline materials formed by hybridization have excellent electrical, optical and mechanical properties. Since its discovery, it has attracted widespread attention from the scientific and industrial circles. Because of the special arrangement of carbon atoms in graphene, its energy band structure is a linearly dispersed Dirac cone, and the effective mass of the carrier is zero, so it has extremely high electron and hole mobility, and gradually Become a strong competitor in silicon-based electronics. On the other hand, the light transmittance of single-layer graphene reaches 97.7%, coupled with its excellent electrical conductivity, it is a very ideal material for a new generation of transparent conductive film...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/02C30B25/18C30B29/64C25F3/22
CPCC25F3/22C30B25/186C30B29/02C30B29/64
Inventor 刘忠范彭海琳林立孙禄钊
Owner PEKING UNIV
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