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Method for preparing graphene film through combination of carbon dioxide and low-pressure chemical vapor deposition

A low-pressure chemical vapor and chemical vapor deposition technology, applied in chemical instruments and methods, graphene, single-layer graphene, etc., can solve the problems of potholes, protrusions and pores, hindering the industrial production of graphene, etc.

Active Publication Date: 2021-06-08
CHIA TAI ENERGY MATERIALS DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing chemical vapor deposition (CVD) growth of graphene must be carried out under normal pressure. In the normal pressure experiment, the surface of the graphene film has pits, bumps and pores, which greatly hinders the industrial production of graphene.

Method used

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  • Method for preparing graphene film through combination of carbon dioxide and low-pressure chemical vapor deposition
  • Method for preparing graphene film through combination of carbon dioxide and low-pressure chemical vapor deposition
  • Method for preparing graphene film through combination of carbon dioxide and low-pressure chemical vapor deposition

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Embodiment 1

[0041] In this embodiment, a graphene film is prepared by chemical vapor deposition under carbon dioxide combined with low pressure, including the following steps:

[0042] (1) Clean the copper foil ultrasonically with acetone, isopropyl ketone, hydrochloric acid and deionized water for 5~10 minutes, then remove the moisture on the surface of the copper foil, then put the copper foil into the quartz tube, and place the copper foil in the tube furnace In the middle, evacuate to below 5 torr, adjust the flow rate of carbon dioxide to 10 sccm, heat the copper foil to 500°C in this atmosphere, and pretreat the gas for 15 minutes. The hydrogen flow rate is 20sccm, and the copper foil is heated to 1000°C in this atmosphere, and annealed for 40 minutes;

[0043] (2) The annealed copper foil in step (1) was fed into methane and hydrogen to grow graphene, wherein the flow rate of carbon dioxide was 8 sccm, the flow rate of methane was 20 sccm and the flow rate of hydrogen was 240 sccm,...

Embodiment 2

[0049]The present embodiment utilizes chemical vapor deposition method to prepare graphene film under low pressure, comprises the following steps:

[0050] (1) Ultrasonic clean the copper foil with acetone, ethanol, ammonium persulfate and deionized water for 5-10 minutes, then remove the moisture on the surface of the copper foil, then put the copper foil into the quartz tube, and make the copper foil in the tube type In the middle of the furnace, evacuate to below 5torr, adjust the flow rate of carbon dioxide to 90sccm, and helium to 10sccm. In this atmosphere, heat the copper foil to 265°C and pretreat the gas for 55 minutes. After the gas pretreatment is completed, cool down to room temperature and adjust the argon The gas flow rate is 100 sccm, the hydrogen gas flow rate is 20 sccm, and the copper foil is heated to 1000°C in this atmosphere environment, and annealed for 40 minutes;

[0051] (2) The annealed copper foil in step (1) was passed through methane and hydrogen t...

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Abstract

The invention discloses a method for preparing a graphene film through combination of carbon dioxide and low-pressure chemical vapor deposition. The method comprises the processes of copper foil pretreatment, copper foil annealing, graphene growth and cooling. Carbon dioxide is adopted to pretreat a copper foil, a copper foil is annealed in a mixed atmosphere of hydrogen and argon at 900-1050 DEG C, a deposition reaction is carried out in a mixed atmosphere of carbon dioxide, hydrogen and methane at 900-1050 DEG C during growth, and argon is adopted for cooling after growth is finished. On the basis of overcoming the defects of a normal-pressure graphene preparation method, carbon dioxide is combined with a low-pressure system to prepare the graphene film, so that the phenomena of pits, bulges, air holes and the like on the surface of the graphene film in a normal-pressure experiment are effectively eliminated, the quality of graphene is improved, the carbon source is wide in source, the cost is reduced, and the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a graphene film, in particular to a method for preparing a graphene film by combining carbon dioxide with low-pressure chemical vapor deposition. Background technique [0002] Graphene is a two-dimensional honeycomb crystal composed of carbon atoms. It has excellent properties in mechanics, heat, optics and electricity, making it suitable for transparent conductive films, sensors, flexible displays and integrated circuits. prospect. [0003] At present, the preparation methods of graphene film mainly include: mechanical exfoliation method, redox method, chemical vapor deposition (CVD), epitaxial growth method and so on. Among them, although the mechanical exfoliation method can produce graphene films with excellent performance, the efficiency is low and the repeatability is poor; the redox method can prepare graphene in large quantities, but its quality is poor and the pressure on environmental protectio...

Claims

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Application Information

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IPC IPC(8): C01B32/186
CPCC01B32/186C01B2204/20C01B2204/02
Inventor 李秀清赵博琪张青龙杨旭王荣海周彤王闯袁龙
Owner CHIA TAI ENERGY MATERIALS DALIAN
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