Method of manufacturing graphene using doped carbon materials

Patent metadata

Field	Value
Publication number	US-10106417-B2
Application number	US-201615393192-A
Country	US
Kind code	B2
Filing date	Dec 28, 2016
Priority date	Dec 30, 2015
Publication date	Oct 23, 2018
Grant date	Oct 23, 2018

Abstract

Provided is a method of manufacturing graphene by unzipping doped carbon materials by an external stimulus and a graphene manufactured therefrom.

First claim

What is claimed is:

1. A method of manufacturing graphene comprising:
i) depositing a metal catalyst on a substrate;
ii) after step i), growing doped carbon materials on the metal catalyst;
iii) after step ii), etching the substrate with an etchant to separate the doped carbon materials;
iv) after step iii), transferring the doped carbon materials to an electrode and then heat-treating the electrode to attach the doped carbon materials to the electrode; and
v) after step iv), putting the electrode, to which the doped carbon materials are attached, in an electrolyte including an oxidizer and applying a voltage to the electrode to perform an oxidation reaction,
wherein the graphene has an edge formed with carbonyl and satisfies the following Formulas 2 to 5 in C1s spectrum obtained by an X-ray photoelectron spectroscopy (XPS):
0.01≤ X 2 /X 1 ≤0.15  [Formula 2]

0.01≤ X 3 /X 1 ≤0.2  [Formula 3]

0.01≤ X 4 /X 1 ≤0.1  [Formula 4]

0.5≤ X 3 /X 2 ≤1,000  [Formula 5]

wherein X 1 represents a peak area of carbon-carbon double bonding, X 2 represents a peak area of carbon-oxygen single bonding, X 3 represents a peak area of carbon-oxygen double bonding, and X 4 represents a peak area of a carboxyl.

2. The method of claim 1 , wherein the oxidizer is at least any one or two selected from sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, hydrofluoric acid, salts thereof, and an aqueous solution thereof.

3. The method of claim 1 , wherein the voltage ranges from 0.01 to 5.0 V.

4. The method of claim 1 , wherein the method further includes:
vi) applying a physical external stimulus to the oxidized carbon materials after step v).

5. The method of claim 2 , wherein the oxidizer is sulfuric acid or sulfuric acid solution.

6. The method of claim 5 , wherein a concentration of the sulfuric acid solution ranges from 0.001 to 10 M.

7. The method of claim 1 , wherein the doped carbon materials are doped with a hetero atom of at least any one selected from nitrogen, phosphorus, arsenic, antimony, bismuth, boron, aluminum, gallium, indium, and thallium.

8. The method of claim 7 , wherein the hetero atom doped on the doped carbon materials is coordinately bonded to at least one metal element.

9. The method of claim 8 , wherein the at least one metal element is at least any one or two selected from Fe, Ni, Cu, W, V, Cr, Sn, Co, Mn, Mo, Mg, Al, Si, Zr, Ti, Ru, Pt, Ag, Au, Pd, Rh, Ir, Ta, Nb, Zn, and Cd.

10. The method of claim 7 , wherein the doped carbon materials are doped at an element ratio that is 0.001 to 10% of the hetero atom with respect to the entire carbon atom.

11. The method of claim 1 , wherein the doped carbon materials are at least any one or two selected from single-walled carbon nanotube, double-walled carbon nanotube, triple-walled carbon nanotube, multi-walled carbon nanotube, and superfine carbon nanotube.

12. The method of claim 1 , wherein the substrate is made of silicon or silicon dioxide.

Assignees

• Korea Advanced Inst Sci & Tech

Inventors

• Kim Sang Ouk
• LIM Joonwon
• Lee Ho Jin

Classifications

• C01B32/184 Primary

  Preparation · CPC title

• C01B32/23

  Oxidation · CPC title

• C01B31/043 Primary

  Chemistry & Metallurgy · mapped topic