Method of preparing graphene and anode mixture for lithium secondary battery including graphene prepared thereby

Patent metadata

Field	Value
Publication number	US-9634329-B2
Application number	US-201414539269-A
Country	US
Kind code	B2
Filing date	Nov 12, 2014
Priority date	Nov 14, 2013
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

Abstract

Disclosed herein is a method of preparing porous graphene from porous graphite, including 1) thermochemically reacting a highly crystalline carbide compound with a halogen element-containing gas to give a porous carbide-derived carbon; 2) treating the carbide-derived carbon with an acid, thus preparing a carbide-derived carbon oxide; and 3) reducing the carbide-derived carbon oxide. An anode mixture for a secondary battery including the graphene and an anode for a secondary battery including the anode mixture are also provided.

First claim

What is claimed is:

1. A method of preparing graphene, comprising:
1) thermochemically reacting a crystalline carbide compound with a halogen element-containing gas to give a porous carbide-derived carbon;
2) treating the carbide-derived carbon with an acid, thus preparing a carbide-derived carbon oxide; and
3) reducing the carbide-derived carbon oxide;
wherein 3) is performed by irradiating a blend of the carbide-derived carbon oxide and a thermal conductor with microwaves so as to be reduced.

2. The method of claim 1 , wherein the carbide compound in 1) is a compound of carbon and any element selected from the group consisting of Groups 3, 4, 5 and 6 elements in periodic table and combinations thereof.

3. The method of claim 2 , wherein the carbide compound comprises at least one selected from the group consisting of SiC, B x C y , TiC, ZrC x , Al x C y , Ca x C y , Ti x Ta y C, Mo x W y C, TiN x C y , ZrN x C y , SiC 4 , TiAlC and Mo 2 C (in which x and y are determined stoichiometrically).

4. The method of claim 1 , wherein the halogen element-containing gas in 1) is selected from the group consisting of Cl 2 , TiCl 4 and F 2 .

5. The method of claim 1 , wherein thermochemically reacting in 1) is performed at 200 to 1200° C.

6. The method of claim 1 , wherein thermochemically reacting in 1) is performed for 3 to 5 hr.

7. The method of claim 1 , further comprising performing annealing with any one gas selected from the group consisting of H 2 , Ar, N 2 and NH 3 , after thermochemically reacting in 1).

8. The method of claim 7 , wherein the annealing is performed for 1 to 3 hr.

9. The method of claim 1 , wherein treating the carbide-derived carbon with the acid in 2) is performed by oxidizing the carbide-derived carbon with an acid solution and an oxidant.

10. The method of claim 9 , wherein the acid solution comprises one or more selected from the group consisting of sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid.

11. The method of claim 9 , wherein the oxidant is hydrogen peroxide or potassium permanganate.

12. The method of claim 1 , wherein the thermal conductor is super-P.

Assignees

• Korea Energy Research Inst

Inventors

• Yeon Sun-Hwa
• Shin Kyoung-Hee
• Jin Chang-Soo
• Jung Kyu-Nam
• Jeon Jae-Deok
• Shim Joonmok
• Yang Jung-Hoon
• Lee Bum-Suk
• Jeon Myung Seok
• Ahn Wook

Classifications

• C01P2006/40

  Electric properties · CPC title

• C01B31/0446

  Chemistry & Metallurgy · mapped topic

• H01M4/587 Primary

  for inserting or intercalating light metals · CPC title

• H01M4/623

  fluorinated polymers · CPC title

• C01B32/184

  Preparation · CPC title