IP Library Granted Patent US 8,173,095
Granted Patent B2
US 8,173,095 · App. 12/241,555 · Granted May 8, 2012

Method and apparatus for producing graphene oxide layers on an insulating substrate

Assignee: Georgia Tech Research Corporation
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Quick Facts
Patent No.
US 8,173,095
App. No.
12/241,555
Granted
May 8, 2012
Kind
B2
Abstract

In a method of making a functionalized graphitic structure, a portion of a multi-layered graphene surface extending from a silicon carbide substrate is exposed to an acidic environment so as to separate graphene layers in a portion of the multi-layered graphene surface. The portion of the multi-layered graphene surface is exposed to a functionalizing material that binds to carbon atoms in the graphene sheets so that the functionalizing material remains between the graphene sheets, thereby generating a functionalized graphitic structure. The functionalized graphitic structure is dried in an inert environment.

Claims (43)

1. A method of making a functionalized graphitic structure, comprising the actions of:

a. exposing a portion of a multi-layered graphene surface extending from a silicon carbide substrate to an acidic environment so as to separate graphene layers in a portion of the multi-layered graphene surface;

b. exposing the portion of the multi-layered graphene surface to a functionalizing material that binds to carbon atoms in the graphene sheets so that the functionalizing material remains between the graphene sheets, thereby generating a functionalized graphitic structure;

c. drying the functionalized graphitic structure in an inert environment;

d. subjecting a portion of the functionalized graphitic structure to a reducing environment; and

e. applying a second masking material that resists the reducing environment to a portion of the functionalized graphitic structure prior to the action of subjecting the portion of the functionalized graphitic structure to the reducing environment.

2. The method of claim 1 , wherein the action of exposing a portion of the graphitic surface to an acidic environment comprises the actions of:

a. submerging the portion of the graphitic surface into a solution of sulfuric acid and sodium nitrate; and

b. maintaining the solution at a temperature that is not greater than 20° C.

3. The method of claim 1 , wherein the action of exposing the portion of the graphitic surface to a functionalizing material comprises the actions of:

a. submerging the portion of the graphitic surface into a solution that includes an oxidizing agent;

b. maintaining the solution at a temperature that is not greater than 20° C.; and

c. agitating the solution.

4. The method of claim 3 , wherein the oxidizer comprises potassium permanganate.

5. The method of claim 4 , further comprising the action of rinsing the portion of the multi-layered graphene surface in water.

6. The method of claim 3 , further comprising the actions of:

a. heating the solution to a temperature that is greater than 32° C. and agitating the solution until visually perceived effervescence of the solution diminishes;

b. adding water to the solution and allowing the solution to increase in temperature until the temperature of the solution is at least 95° C. and maintaining the solution at a temperature of at least 95° C. for at least one minute; and

c. adding a solution of water and hydrogen peroxide to the solution, thereby terminating the reaction.

7. The method of claim 1 , wherein the inert environment comprises a nitrogen flow.

8. The method of claim 1 , further comprising the action of applying a first masking material to a portion of the multi-layered graphene surface prior to exposing the portion of the multi-layered graphene surface to an acidic environment, the mask material configured to inhibit contact between the portion of the multi-layered graphene surface and the acidic environment, thereby generating a patterned functionalized graphitic structure.

9. The method of claim 8 , wherein the first masking material comprises a material selected from a group consisting of hydrogen silsesquioxane and SU-8 photoresist.

10. The method of claim 1 , wherein the action of subjecting a portion of the functionalized graphitic structure to a reducing environment comprises applying an energy source to the portion of the functionalized graphitic structure.

11. The method of claim 1 , wherein the action of subjecting a portion of the functionalized graphitic structure to a reducing environment comprises the action of applying an electron beam to the portion of the functionalized graphitic structure.

12. A method of making a functionalized graphitic structure, comprising the actions of:

a. exposing a portion of a multi-layered graphene surface extending from a silicon carbide substrate to an acidic environment so as to separate graphene layers in a portion of the multi-layered graphene surface, wherein the action of exposing the portion of the graphitic surface to a functionalizing material comprises the actions of:

i. submerging the portion of the graphitic surface into a solution that includes an oxidizing agent;

ii. maintaining the solution at a temperature that is not greater than 20° C.; and

iii. agitating the solution;

b. exposing the portion of the multi-layered graphene surface to a functionalizing material that binds to carbon atoms in the graphene sheets so that the functionalizing material remains between the graphene sheets, thereby generating a functionalized graphitic structure, wherein the exposing the portion of the multi-layered graphene surface to a functionalizing material, comprises the actions of:

i. heating the solution to a temperature that is greater than 32° C. and agitating the solution until visually perceived effervescence of the solution diminishes;

ii. adding water to the solution and allowing the solution to increase in temperature until the temperature of the solution is at least 95° C. and maintaining the solution at a temperature of at least 95° C. for at least one minute; and

iii. adding a solution of water and hydrogen peroxide to the solution, thereby terminating the reaction; and

c. drying the functionalized graphitic structure in an inert environment.

13. The method of claim 12 , further comprising the action of subjecting a portion of the functionalized graphitic structure to a reducing environment.

14. The method of claim 12 , wherein the action of exposing a portion of the graphitic surface to an acidic environment comprises the actions of:

a. submerging the portion of the graphitic surface into a solution of sulfuric acid and sodium nitrate; and

b. maintaining the solution at a temperature that is not greater than 20° C.

15. The method of claim 12 , wherein the action of exposing the portion of the graphitic surface to a functionalizing material comprises the actions of:

c. submerging the portion of the graphitic surface into a solution that includes an oxidizing agent;

d. maintaining the solution at a temperature that is not greater than 20° C.; and

e. agitating the solution.

16. The method of claim 12 , further comprising the action of applying a first masking material to a portion of the multi-layered graphene surface prior to exposing the portion of the multi-layered graphene surface to an acidic environment, the mask material configured to inhibit contact between the portion of the multi-layered graphene surface and the acidic environment, thereby generating a patterned functionalized graphitic structure.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jan 3, 2011
From: GEORGIA TECH RESEARCH CORPORATION
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 025574/0412 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 30, 2008
From: DE HEER, WALT A.; WU, XIAOSONG; SPRINKLE, MICHAEL; BERGER, CLAIRE
To: GEORGIA TECH RESEARCH CORPORATION
Reel/Frame 022041/0470 →
Continuity (2)
Provisional Application 61037585 · Mar 18, 2008
Related Publication 20090236609A1 · Sep 24, 2009