Dissolution of graphite, graphite and graphene nanoribbons in superacid solutions and manipulation thereof

Patent metadata

Field	Value
Publication number	US-9534319-B2
Application number	US-201013202352-A
Country	US
Kind code	B2
Filing date	Feb 19, 2010
Priority date	Feb 19, 2009
Publication date	Jan 3, 2017
Grant date	Jan 3, 2017

Abstract

Methods for dissolving carbon materials such as, for example, graphite, graphite oxide, oxidized graphene nanoribbons and reduced graphene nanoribbons in a solvent containing at least one superacid are described herein. Both isotropic and liquid crystalline solutions can be produced, depending on the concentration of the carbon material The superacid solutions can be formed into articles such as, for example, fibers and films, mixed with other materials such as, for example, polymers, or used for functionalization of the carbon material. The superacid results in exfoliation of the carbon material to produce individual particles of the carbon material. In some embodiments, graphite or graphite oxide is dissolved in a solvent containing at least one superacid to form graphene or graphene oxide, which can be subsequently isolated. In some embodiments, liquid crystalline solutions of oxidized graphene nanoribbons in water are also described.

First claim

What is claimed is the following:

1. A method comprising:
dissolving graphite oxide in a solvent to form a solution,
wherein the solvent comprises at least one superacid,
wherein the dissolving comprises mixing the graphite oxide in the solvent, and
wherein the mixing results in exfoliation of the graphite oxide to form an oxidized graphene in the solution.

2. The method of claim 1 , further comprising:
removing the solvent; and
isolating the oxidized graphene.

3. The method of claim 1 , wherein the mixing comprises high shear mixing the graphite oxide in the solvent.

4. The method of claim 1 , wherein the mixing comprises sonicating the graphite oxide in the solvent.

5. The method of claim 1 , wherein the oxidized graphene comprises from about one layer to about ten layers.

6. The method of claim 1 , further comprising:
providing the graphite oxide.

7. The method of claim 1 , wherein the mixing comprises stirring the graphite oxide in the solvent.

8. The method of claim 1 , wherein the solvent comprises chlorosulfonic acid.

9. The method of claim 1 , wherein the solvent comprises at least chlorosulfonic acid and sulfuric acid.

10. The method of claim 1 , further comprising:
centrifuging the solution; and
separating the solution from any undissolved graphite oxide.

11. The method of claim 1 , further comprising:
mixing the solution with a polymer; and
removing the solvent from the polymer to form a composite material;
wherein the composite material comprises the polymer and the oxidized graphene.

12. The method of claim 1 , further comprising:
forming an article from the solution;
wherein the article comprises a neat form of the oxidized graphene; and
removing the solvent from the article.

13. The method of claim 12 , wherein forming comprises a process selected from the group consisting of extruding the solution through a spinneret, extruding the solution through a needle, extruding the solution through a film die, spreading the solution into a film, casting the solution into a mold, and combinations thereof.

14. The method of claim 12 , wherein removing comprises a process selected from the group consisting of coagulation, evaporation, heating under vacuum and combinations thereof.

15. The method of claim 1 , further comprising:
functionalizing the graphite oxide while in the solution.

16. The method of claim 1 , wherein the formed solution is an isotropic solution.

17. The method of claim 16 , further comprising:
mixing the solution with a polymer; and
removing the solvent from the polymer to form a composite material;
wherein the composite material comprises the polymer and the oxidized graphene.

18. The method of claim 16 , further comprising:
depositing the solution on a surface; and
removing the solvent to form a film comprising the oxidized graphene on the surface.

19. The method of claim 16 , further comprising:
functionalizing the graphite oxide while in the solution.

20. The method of claim 1 , wherein the formed solution is a liquid crystalline solution.

21. The method of claim 20 , further comprising:
forming an article from the solution;
wherein the article comprises a neat form of the oxidized graphene; and

removing the solvent from the article.

22. The method of claim 21 , wherein forming comprises a technique selected from the group consisting of extruding the solution through a spinneret, extruding the solution through a needle, extruding the solution through a film die, spreading the solution into a film, casting the solution into a mold, and combinations thereof.

23. The method of claim 21 , wherein removing comprises a process selected from the group consisting of coagulation, evaporation, heating under vacuum and combinations thereof.

Assignees

• Tour James M
• Pasquali Matteo
• Behabtu Natnael
• Lomeda Jay R
• Kosynkin Dmitry V
• Duque Amanda
• Green Micah J
• Parra-Vasquez A Nicholas
• Young Colin
• Univ Rice William M

Inventors

• Tour James M
• Pasquali Matteo
• Behabtu Natnael
• Lomeda Jay R
• Kosynkin Dmitry V
• Duque Amanda
• Green Micah J
• Parra-Vasquez A Nicholas
• Young Colin

Classifications

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• D01F9/12

  Carbon filaments; Apparatus specially adapted for the manufacture thereof · CPC title

• C01B32/194

  After-treatment · CPC title

• D01D5/04

  Dry spinning methods {(D01D5/0038 takes precedence)} · CPC title