Process for preparing graphene on a SiC substrate based on metal film-assisted annealing

Patent metadata

Field	Value
Publication number	US-9691612-B2
Application number	US-201214369780-A
Country	US
Kind code	B2
Filing date	Sep 3, 2012
Priority date	Jan 3, 2012
Publication date	Jun 27, 2017
Grant date	Jun 27, 2017

Abstract

Provided is a process for preparing graphene on a SiC substrate, based on metal film-assisted annealing, comprising the following steps: subjecting a SiC substrate to a standard cleaning process; placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150° C.; introducing CCl 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CCl 4 vapor is carried by Ar gas; forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition; placing the obtained double-layered carbon film sample onto the metal film; subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100° C. for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and removing the metal film from the double-layered graphene, thereby obtaining double-layered graphene. Also provided is double-layered graphene prepared by said process.

First claim

What is claimed is:

1. A process for preparing graphene on a SiC substrate, based on metal film-assisted annealing, comprising the following steps:
(1) subjecting a SiC substrate to a standard cleaning process so as to remove contaminants from the surface of the SiC substrate;
(2) placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150° C.; and introducing CCl 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CCl 4 vapor is carried by Ar gas;
(3) forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition, wherein the metal film is capable of catalyzing carbon to reconstitute into graphene;
(4) placing the obtained double-layered carbon film sample onto the metal film, and subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100° C. for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and
(5) removing the metal film from the double-layered graphene, and thereby obtaining double-layered graphene.

2. The process for preparing graphene according to claim 1 , characterized in that step (1) subjecting a SiC substrate to a standard cleaning process is carried out by:
(1a) immersing the SiC substrate in a medium of NH 4 OH+H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove organic residues from the surface of the SiC substrate; and
(1b) immersing the SiC substrate in a medium of HCl+H 2 O 2 for 1 minutes, taking the SiC substrate out and drying it so as to remove ionic contaminants.

3. The process for preparing graphene according to claim 1 , characterized in that the flow rate of Ar gas in step (2) is 40 to 90 ml/min.

4. The process for preparing graphene according to claim 1 , characterized in that the electron beam deposition in step (3) is carried out under the following conditions: the distance between the SiC substrate and the target being 50 cm, the chamber pressure being 5×10 −4 Pa, the beam current being 40 mA, and the evaporation time being 10 to 20 minutes.

5. The process for preparing graphene according to claim 1 , characterized in that the flow rate of Ar gas during annealing in step (4) is 20-100 ml/min.

6. The process for preparing graphene according to claim 1 , characterized in that the SiC substrate is in a crystal form of 4H—SiC or 6H—SiC.

7. The process for preparing graphene according to claim 1 , characterized in that the CCl 4 vapor in step (2) is obtained by heating CCl 4 liquid to a temperature of 60 to 90° C.

8. The process for preparing graphene according to claim 1 , characterized in that the metal film is a Ni film.

Assignees

• Guo Hui
• Zhang Keji
• Zhang Yuming
• Deng Pengfei
• Lei Tianmin
• Univ Xidian

Inventors

• Guo Hui
• Zhang Keji
• Zhang Yuming
• Deng Pengfei
• Lei Tianmin

Classifications

• H10P14/3602

  In-situ cleaning · CPC title

• H10P14/3406

  Carbon, e.g. diamond-like carbon · CPC title

• H10P14/2904

  Silicon carbide · CPC title

• H10P14/38

  characterised by treatments done after the formation of the materials · CPC title

• H10P14/203 Primary

  using transformation of metal, e.g. oxidation or nitridation · CPC title