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Method for preparing graphene through chemical vapor deposition under cold cavity wall condition

A chemical vapor deposition and graphene technology, which is applied in the field of graphene preparation, can solve the problems of unfavorable high-quality graphene, the influence of graphene growth quality, and the increase of heating area

Inactive Publication Date: 2011-04-06
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of graphene by chemical vapor deposition mostly adopts the hot wall method, that is, the synthesis of graphene occurs in a quartz tube furnace. 【7】-【10】 , the hot chamber wall will lead to an increase in the area of ​​the heating area, resulting in the decomposition of more carbon-containing source gas, which is not conducive to the synthesis of high-quality graphene; secondly, the carbon-containing source gas decomposed near the hot wall is adsorbed on the hot wall to form Carbon particles, carbon particles fall on the surface of the substrate where graphene grows, affecting the growth quality of graphene

Method used

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  • Method for preparing graphene through chemical vapor deposition under cold cavity wall condition
  • Method for preparing graphene through chemical vapor deposition under cold cavity wall condition
  • Method for preparing graphene through chemical vapor deposition under cold cavity wall condition

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Embodiment 1

[0035] The method of this embodiment 1 is to place the copper foil substrate with an area of ​​10 mm × 10 mm, a thickness of 25 μm, and argon plasma treatment on the surface on the heating table of the chemical vapor deposition equipment; open the circulating water to cool the cavity wall to 25 ℃; vacuumize, so that the background vacuum of the cavity reaches below 3mTorr; feed the mixed gas of nitrogen (purity 99.999%) and hydrogen (purity 99.999%), nitrogen flow is 700sccm, hydrogen flow is 100sccm, and starts to heat up at a rate of 100°C / min, the chamber pressure is 3Torr; after the substrate temperature reaches 1000°C and is kept warm for 30 minutes, methane gas (purity 99.99%) is introduced, the flow rate is 30sccm, and the duration is 30 minutes; set the substrate cooling rate to 200°C / min, cool down the substrate and stop feeding methane gas; wait for the substrate to cool down to room temperature, stop feeding hydrogen and nitrogen. Graphene can be obtained after the ...

Embodiment 2

[0037] The method of this embodiment 2 is to place the substrate of nickel / silicon dioxide / silicon structure with an area of ​​10mm×10mm on the heating table of the chemical vapor deposition equipment, wherein the thicknesses of nickel, silicon dioxide and silicon are respectively 300nm and 300nm and 0.5mm; open the circulating water to cool the cavity wall to 25°C; vacuumize the cavity to make the background pressure of the cavity reach 150Torr; only feed nitrogen (purity 99.999%), the nitrogen flow rate is 500sccm, and start to heat up at a rate of 100°C / min, the cavity pressure is 15Torr; after the substrate temperature reaches 1000°C and is kept for 30 minutes, methane gas (purity 99.99%) is introduced, the flow rate is 8sccm, and the duration is 10 seconds; the substrate cooling rate is set to 200°C / min, cool down the substrate and stop feeding methane gas; wait for the substrate to cool down to room temperature, stop feeding hydrogen and nitrogen. Graphene can be obtaine...

Embodiment 3

[0039] The method of this embodiment 3 is to place the substrate of the iron-platinum alloy film / silicon structure with an area of ​​20mm×20mm on the heating table of the chemical vapor deposition equipment, wherein the thicknesses of the iron-platinum alloy film and the silicon wafer are respectively 200nm and 0.5mm ; Turn on the circulating water to cool the chamber wall to 25°C; vacuumize the chamber so that the background pressure of the chamber reaches 3Torr; feed the mixed gas of helium (purity 99.999%) and hydrogen (purity 99.999%), and the helium flow rate is 600sccm, the flow rate of hydrogen gas is 50sccm, and the temperature starts to rise at a rate of 100°C / min, and the pressure of the chamber is 750Torr; after the substrate temperature reaches 750°C and is kept for 20 minutes, acetylene (purity 99.8%) is started, and the flow rate is 50sccm, which lasts The time is 10 minutes; set the cooling rate of the substrate to 200°C / min, cool down the substrate and stop feed...

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Abstract

The invention discloses a method for preparing graphene through chemical vapor deposition under a cold cavity wall condition. The method comprises the following detailed steps of: 1) placing a substrate in a sealed cavity with circulating water cooling, wherein the temperature of the cavity wall is controlled to be between the room temperature and 100 DEG C; 2) introducing carrier gas and heatingthe substrate; 3) continuously introducing carbon source-containing gas for 5 to 30 seconds; and 4) after cooling the substrate, generating the grapheme on the surface of the substrate. When the coldcavity wall chemical vapor deposition is compared with the traditional widely used hot cavity wall chemical vapor deposition, the heated area is only limited to the substrate and the other parts of the cavity are cooled, so that the decomposition of the carbon source-containing gas can be reduced, the growing thickness of the grapheme is precisely controlled, and carbon can deposit on the surfaceof the substrate in a form of a single atom layer to generate the single-layer grapheme. The grapheme prepared by the method has the advantages of good uniformity, large area, few defects, excellent electricity conductivity, good mechanical properties and the like.

Description

technical field [0001] The invention relates to a method for preparing graphene, more specifically a method for directly preparing graphene by chemical vapor deposition under cold chamber wall conditions. Background technique [0002] Graphene, a new type of material with two-dimensional carbon nanostructure, shows excellent thermal, mechanical and electrical properties macroscopically due to its unique nanostructure, and has become a scientific research object in recent years. Research Hotspots 【1】 . The excellent properties shown by graphene make it have a wide range of application prospects, such as displays, solar cells and supercapacitors, etc. 【2】 . However, it is still difficult to grow large-area, high-quality graphene, which makes this material not meet the requirements of industrial applications. [0003] At present, the preparation methods of graphene at home and abroad include: redox method of graphite 【3】 , silicon sublimation method of silicon carbide 【4】...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 黄磊常全鸿纪乐春刘洋郭桂略王涛
Owner SHANGHAI NORMAL UNIVERSITY
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