IP Library Granted Patent US 9,422,165
Granted Patent B2
US 9,422,165 · App. 14/397,302 · Granted Aug 23, 2016

Graphene compositions and methods of making the same

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Quick Facts
Patent No.
US 9,422,165
App. No.
14/397,302
Granted
Aug 23, 2016
Kind
B2
Abstract

Compositions comprising graphene and methods for preparing graphene are described.

Claims (28)

1. A method of preparing graphene, the method comprising:

contacting a graphitic oxide composition with a photocatalytic-coated metal substrate or a photocatalytic-coated silicon wafer to yield graphene, wherein the graphitic oxide composition comprises graphitic oxide and an organic solvent.

2. The method of claim 1 , the method further comprising preparing the graphitic oxide composition, the method of preparing the graphitic oxide composition comprising:

dissolving graphite in a concentrated acid to produce an graphite-acid solution;

contacting the graphite-acid solution with a nitrate or salt thereof to yield a graphite-acid-nitrate solution;

contacting the graphite-acid-nitrate solution with an oxidizer to yield the graphitic oxide;

purifying the graphitic oxide; and

dissolving the purified graphitic oxide in the organic solvent to produce the graphitic oxide composition.

3. The method of claim 2 , wherein the oxidizer is hydrogen peroxide, hydrazine, persulfuric acid, perchlorate, hypochlorite, or any combination thereof.

4. The method of claim 2 , wherein the nitrate is potassium nitrate, ammonium nitrate, sodium nitrate, or any combination thereof.

5. The method of claim 2 , wherein the acid is sulfuric acid, nitric oxide, or any combination thereof.

6. The method of claim 2 , wherein the graphite is dissolved in a concentrated acid at a pH of less than or equal to 2.0.

7. The method of claim 2 , wherein the graphite-acid solution is contacted with a nitrate or salt thereof in an ice bath to yield the graphite-acid-nitrate solution.

8. The method of claim 2 , wherein the graphitic oxide is purified by filtering the graphitic oxide to yield purified graphitic oxide.

9. The method of claim 1 , wherein the organic solvent is toluene, ethyl acetate, glycol ether, acetone, or any combination thereof.

10. The method of claim 1 , wherein the graphitic oxide composition is coated on the photocatalytic coated metal substrate or the photocatalytic-coated silicon wafer.

11. The method of claim 10 , wherein the photocatalytic coated metal substrate or the photocatalytic-coated silicon wafer is coated with the graphitic oxide composition by spin coating the photocatalytic coated metal substrate or the photocatalytic-coated silicon wafer with the graphitic oxide composition.

12. The method of claim 1 , wherein the photocatalytic is Pd/WO 3 , ZnO, Ru, TiO 2 , Pt, or any combination thereof.

13. The method of claim 1 , wherein the metal substrate is an aluminum substrate, copper substrate, silver substrate, iron substrate, zinc substrate, or any combination thereof.

14. The method of claim 1 , further comprising heating the graphitic oxide composition and the photocatalytic-coated metal substrate or the photocatalytic-coated silicon wafer to a temperature of about 45° C. to 85° C.

15. The method of claim 14 , wherein the graphitic oxide composition and the photocatalytic-coated metal substrate or the photocatalvtic-coated silicon wafer is heated to the temperature of about 45° C. to 85° C. at a rate of about 5° C. per minute.

16. The method of claim 14 , wherein the graphitic oxide composition and the photocatalytic-coated metal substrate or the photocatalvtic-coated silicon wafer is maintained at a temperature of about 45° C. to 85° C. for about 5 to about 20 minutes.

17. The method of claim 1 , wherein the graphitic oxide composition is reacted with a photocatalytic coated metal substrate or the photocatalvtic-coated silicon wafer by exposing the graphitic oxide composition and the photocatalytic-coated metal substrate or the photocatalytic-coated silicon wafer to light to yield the graphene.

18. The method of claim 17 , wherein the graphitic oxide composition is reacted with the photocatalytic-coated metal substrate or the photocatalvtic-coated silicon wafer by contacting the graphitic oxide and the photocatalytic-coated metal substrate or the photocatalytic-coated silicon wafer with oxygen (O 2 ) in the presence of an inert gas at a temperature of about 45° C. to 85° C.

19. The method of claim 1 , further comprising isolating the graphene.

20. The method of claim 1 , wherein the graphene is a sheet of graphene.

21. The method of claim 1 , wherein the graphene has high electrical conductivity.

22. The method of claim 1 , wherein the graphitic oxide composition is graphic oxide dissolved in the organic solvent.

Assignments (2)
SECURITY INTEREST Recorded Jan 29, 2019
From: EMPIRE TECHNOLOGY DEVELOPMENT LLC
To: CRESTLINE DIRECT FINANCE, L.P.
Reel/Frame 048373/0217 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 15, 2015
From: THEVASAHAYAM, AROCKIADOSS
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 035837/0641 →