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Method for growing graphene film by using low-temperature chemical vapor deposition

A graphene film and vapor deposition technology, applied in chemical instruments and methods, from chemically reactive gases, crystal growth, etc., can solve the problems of lowering the temperature of growing graphene, poor quality of graphene, and non-continuous graphene film, etc. Achieve the effect of reducing nucleation density, increasing single crystal size and reducing roughness

Active Publication Date: 2013-07-03
WUXI GRAPHENE FILM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The growth temperature of graphene using Au-Ni alloy catalyst can be as low as 450°C, but only 74% of single-layer graphene can be obtained, and Raman spectrum shows that at the grain boundary, the D peak (peak) is significantly higher than the G peak (low peak), poor graphene quality
[0005] Using carbon-containing liquid as a carbon source can also reduce the temperature for growing graphene. It has been reported that benzene was used as a carbon source to grow graphene at 300°C by low-pressure chemical vapor deposition (LPCVD). Unfortunately, the obtained graphene film is not Continuous, difficult to meet the requirements of use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A method for growing high-quality graphene films by low-temperature chemical vapor deposition, comprising the following steps:

[0054] (1) Take 4 inches of copper foil with a purity of 99.8% as the substrate for growing graphene, put the copper foil into the polishing solution, polish it at a voltage of 3V for 90 seconds, turn off the power, and clean the copper foil;

[0055] (2) Evenly spin-coat the nickel chloride solution with a concentration of 0.01M on the surface of the copper foil, and leave it for a period of time to completely dry the surface of the copper foil;

[0056] (3) Put the above-mentioned surface-doped copper foil into the center of the atmosphere tube furnace, feed nitrogen and hydrogen into the tube furnace, raise the temperature to 1000°C and keep it for 30 minutes, and anneal the copper foil;

[0057] (4) Lower the temperature to 700°C, feed methane into the tube furnace, control the flow rate of methane to 10 sccm and maintain the growth temper...

Embodiment 2

[0060] A method for growing high-quality graphene films by low-temperature chemical vapor deposition, comprising the following steps:

[0061] (1) Take 4 inches of copper foil with a purity of 99.8% as the substrate for growing graphene, and mechanically polish the copper foil on a rotary surface polishing machine with a rotation speed of 3000rpm;

[0062] (2) Chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) The solution is evenly spin-coated on the surface of the copper foil, and left for a period of time to completely dry the surface of the copper foil;

[0063] (3) Put the above-mentioned surface-doped copper foil into the center of the atmosphere tube furnace, feed argon and hydrogen into the tube furnace, raise the temperature to 950°C and keep it for 60 minutes, and anneal the copper foil;

[0064] (4) Lower the temperature to 650°C, feed ethylene into the tube furnace, control the flow of ethylene to 20 sccm and maintain the growth temperature for 45 minutes, and form a grap...

Embodiment 3

[0067] A method for low-temperature growth of high-quality graphene films, comprising the following steps:

[0068] (1) Take a 3.5-inch metal nickel as the substrate for growing graphene, put the metal nickel into the polishing solution, polish it at a voltage of 5V for 30 seconds, turn off the power, and clean the metal nickel;

[0069] (2) Evenly spin-coat the copper chloride solution with a concentration of 0.1M on the surface of the nickel metal, and leave it for a period of time to completely dry the surface of the nickel metal;

[0070] (3) Put the metal nickel doped on the above surface into the center of the atmosphere tube furnace, pass hydrogen gas into the tube furnace, raise the temperature to 600°C and keep it for 30min, and anneal the metal nickel;

[0071] (4) Lower the temperature to 550°C, feed methane into the tube furnace, control the flow rate of methane to 5 sccm and maintain the growth temperature for 90 min, and form a graphene film on the surface of met...

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Abstract

The invention relates to a method for preparing a graphene film in a low-temperature condition. The method at least comprises the following steps: (1), performing smooth treatment on a metal substrate; (2), performing doping of a chemical reagent on the surface of the metal substrate obtained in the step (1); (3), under a protective atmosphere, performing annealing treatment on the metal substrate obtained in the step (1); (4), contacting the metal substrate with a carbon source, and performing chemical vapor deposition in the low-temperature condition to obtain the graphene film; and optionally, after the step (4), performing step (5), stopping heating, cooling to the room temperature, and taking out the metal substrate with the graphene film thereon, wherein the chemical reagent is a precursor salt of metal. The method for growing the graphene film is low in growth temperature, low in cost, high in industrialized feasibility and wide in select range of the substrate, and can prepare the complete single-layer or multi-layer graphene film with high quality.

Description

technical field [0001] The invention relates to a method for growing a graphene film by low-temperature chemical vapor deposition, and belongs to the field of graphene electronic film materials. Background technique [0002] Graphene is a hexagonal honeycomb-shaped two-dimensional nanomaterial composed of sp2 hybridized carbon atoms. At present, the preparation methods of free-state graphene can be roughly divided into physical methods and chemical methods. Physical methods include micromechanical exfoliation method, epitaxial growth method, epitaxial growth method, etc.; chemical methods include graphite oxide reduction method, chemical vapor deposition method, etc. . Among them, the chemical vapor deposition method can obtain graphene with large area and uniform thickness. Regarding the preparation of graphene, the preparation of large-scale graphene films, and the transfer of large-scale graphene films, those skilled in the art have done some research. Preparation of G...

Claims

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Application Information

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IPC IPC(8): C23C16/02C23C16/26C30B25/00C30B29/02
Inventor 黄孟琼
Owner WUXI GRAPHENE FILM
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