IP Library Granted Patent US 8,728,578
Granted Patent B2
US 8,728,578 · App. 13/106,498 · Granted May 20, 2014

Chemical synthesis for graphene sheets greater than 1 μm in length

Inventors: Miriam Rafailovich (Plainview, NY); Rebecca Isseroff (West Hempstead, NY); Paul Masih Das (Lawrence, NY)
Assignee: The Research Foundation for the State University of New York
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Quick Facts
Patent No.
US 8,728,578
App. No.
13/106,498
Granted
May 20, 2014
Kind
B2
Abstract

A method for preparing a graphene sheet greater than 1 μm in length that includes: combining graphitic oxide with a solvent having a ratio of from about 50:50 to about 80:20 deionized water and ethanol to form a graphitic oxide solution; mixing a solution of NaBH 4 and deionized water and the graphitic oxide solution to form a mixture having a concentration of from 10 mmolar to 20 mmolar NaBH 4 ; depositing the mixture on a substrate to form a sheet; and heating the mixture at a temperature of from 25° C. to 85° C. for from 3 to 30 minutes.

Claims (28)

1. A method for preparing a graphene sheet greater than 1 μm in length, the method comprising:

combining graphitic oxide with a solvent comprising ethanol and deionized water to form a graphitic oxide solution;

mixing a reductant and the graphitic oxide solution to form a mixture, wherein the reductant is NaBH 4 , and wherein the concentration of the reductant in the mixture is from 5 mmolar to 25 mmolar; and

heating the mixture at a temperature of from 25° C. to 90° C. for from 3 to 30 minutes.

2. The method for preparing a graphene sheet according to claim 1 , wherein the volumetric ratio of deionized water to ethanol is from about 50:50 to about 80:20.

3. The method for preparing a graphene sheet according to claim 1 , wherein the volumetric ratio of deionized water to ethanol is from about 65:35 to about 75:25.

4. The method for preparing a graphene sheet according to claim 1 , wherein the NaBH 4 is mixed with deionized water to form a solution prior to mixing with the graphitic oxide solution.

5. The method for preparing a graphene sheet according to claim 4 , wherein the concentration of the reductant in the mixture is from 10 mmolar to 20 mmolar.

6. The method for preparing a graphene sheet according to claim 4 , wherein the concentration of the reductant in the mixture is less than 15 mmolar.

7. The method for preparing a graphene sheet according to claim 1 , wherein the heating of the mixture is carried out at a temperature of from 50° C. to 85° C.

8. A method for preparing a graphene sheet greater than 1 μm in length, the method comprising:

combining graphitic oxide with a solvent comprising deionized water and ethanol to form a graphitic oxide solution;

mixing a reductant and the graphitic oxide solution to form a mixture, wherein the reductant is NaBH 4 , and wherein the concentration of the reductant in the mixture is from 10 mmolar to 20 mmolar; and

heating the mixture at a temperature of from 50° C. to 85° C. for from 3 to 30 minutes.

9. The method for preparing a graphene sheet according to claim 8 , wherein the volumetric ratio of deionized water to ethanol is from about 50:50 to about 80:20.

10. The method for preparing a graphene sheet according to claim 8 , wherein the volumetric ratio of deionized water to ethanol is from about 65:35 to about 75:25.

11. The method for preparing a graphene sheet according to claim 8 , wherein the NaBH 4 is mixed with deionized water to form a solution prior to mixing with the graphitic oxide solution.

12. The method for preparing a graphene sheet according to claim 11 , wherein the concentration of the reductant in the mixture is less than 15 mmolar.

13. The method for preparing a graphene sheet according to claim 12 , wherein the heating of the mixture is carried out at a temperature of from 75° C. to 85° C.

14. The method for preparing a graphene sheet according to claim 13 , wherein the heating of the mixture is carried out for from 5 to 15 minutes.

15. A method for preparing a graphene sheet greater than 1 μm in length, the method comprising:

combining graphitic oxide with a solvent comprising a first deionized water and ethanol to form a graphitic oxide solution, wherein the volumetric ratio of deionized water to ethanol is from about 50:50 to about 80:20;

mixing a solution of NaBH 4 and a second deionized water and the graphitic oxide solution to form a mixture, wherein the concentration of NaBH 4 in the mixture is from 10 mmolar to 20 mmolar; and

heating the mixture at a temperature of from 25° C. to 90° C. for from 3 to 30 minutes.

16. The method for preparing a graphene sheet according to claim 15 , wherein the volumetric ratio of the first deionized water to ethanol is from about 65:35 to about 75:25.

17. The method for preparing a graphene sheet according to claim 16 , wherein the concentration of the reductant NaBH 4 in the mixture is from 13 mmolar to 17 mmolar.

18. The method for preparing a graphene sheet according to claim 17 , wherein the heating of the mixture is carried out at a temperature of from 75° C. to 85° C.

19. The method for preparing a graphene sheet according to claim 18 , wherein the heating of the mixture is carried out for from 5 to 15 minutes.

Assignments (2)
CHANGE OF NAME Recorded Apr 2, 2014
From: THE RESEARCH FOUNDATION OF STATE UNIVERSITY OF NEW YORK
To: THE RESEARCH FOUNDATION FOR THE STATE UNIVERSITY OF NEW YORK
Reel/Frame 032589/0302 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 21, 2011
From: RAFAILOVICH, MIRIAM; ISSEROFF, REBECCA; DAS, PAUL MASIH
To: THE RESEARCH FOUNDATION OF STATE UNIVERSITY OF NEW YORK
Reel/Frame 026629/0613 →
Continuity (2)
Provisional Application 61334372 · May 13, 2010
Related Publication 20110281035A1 · Nov 17, 2011