IP Library Granted Patent US 10,233,087
Granted Patent B2
US 10,233,087 · App. 14/820,411 · Granted Mar 19, 2019

Highly crystalline 3D graphene

Inventors: Marcus A. Worsley (Hayward, CA); Leta Woo (Atlanta, GA); William Mickelson (Albany, CA); Alex Zettl (Kensington, CA)
Assignees: Lawrence Livermore National Security, LLC; The Regents of the University of California
C01B32/184C01B32/182C01B2204/22C01B2204/32C01P2002/82C01P2006/10C01P2006/12C01P2006/14C01P2006/40
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Quick Facts
Patent No.
US 10,233,087
App. No.
14/820,411
Granted
Mar 19, 2019
Kind
B2
Abstract

Disclosed here is a composition comprising at least one graphene aerogel comprising a three-dimensional structure of graphene sheets, wherein the graphene sheets are covalently interconnected, and wherein the graphene aerogel is highly crystalline. Also described is a method for making a graphene aerogel, comprising preparing a mixture comprising a graphene oxide suspension and at least one catalyst; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel at a temperature of 1500-3500° C. to produce the graphene aerogel.

Claims (24)

1. A composition comprising at least one graphene aerogel comprising a three-dimensional structure of graphene sheets, wherein the graphene sheets are covalently interconnected, wherein the graphene aerogel has a Raman spectra in which I D /I G is 0.7 or less, wherein the graphene aerogel has an electrical conductivity of 200-600 S/m and a density of 80 mg/ml or less, and wherein the graphene aerogel is produced by a process comprising thermal annealing at a temperature of 1500-3500° C.

2. The composition of claim 1 , wherein the graphene aerogel has a Raman spectra in which I G′ /I G is 0.5 or more.

3. The composition of claim 1 , wherein the graphene aerogel has an average crystallite size L a of 30 nm or more.

4. The composition of claim 1 , wherein the graphene aerogel has an electrical conductivity of 300-600 S/m.

5. The composition of claim 1 , wherein the graphene aerogel has an oxidation temperature T O of 700° C. or more.

6. The composition of claim 1 , wherein the graphene aerogel has a Young's modulus of 50 MPa or more.

7. The composition of claim 1 , wherein the graphene aerogel has a density of 60 mg/ml or less.

8. The composition of claim 1 , wherein the graphene aerogel has a BET surface area of 300 m 2 /g or more.

9. The composition of claim 1 , wherein the graphene aerogel has a pore volume of at least 1 cm 3 /g.

10. The composition of claim 1 , wherein pores having a diameter of 100 nm or less account for 50% or more of the total pore volume of the graphene aerogel.

11. The composition of claim 1 , wherein pores having a diameter of 100 nm or less account for 50% or more of the total pore number of the graphene aerogel.

12. The composition of claim 1 , wherein 70% or more of the covalent bonds interconnecting the graphene sheets are sp 2 carbon bonds.

13. The composition of claim 1 , wherein the graphene aerogel has an atomic oxygen content of 5% or less.

14. The composition of claim 1 , wherein the graphene aerogel is in the form of a monolith having at least one lateral dimension of 1 mm or more.

15. The composition of claim 1 , wherein the graphene aerogel consists essentially of covalently interconnected graphene sheets.

16. The composition of claim 1 , wherein the composition does not comprise a macroporous foam.

17. A method for making the graphene aerogel of claim 1 , comprising:

preparing a mixture comprising a graphene oxide suspension and at least one catalyst;

curing the mixture to produce a wet gel;

drying the wet gel to produce a dry gel; and

thermally annealing the dry gel at a temperature of 1500-3500° C. to produce the graphene aerogel.

18. The method of claim 17 , wherein the dry gel is thermally annealed at a temperature of 2000-3000° C.

19. The method of claim 17 , wherein the mixture consists essentially of the graphene oxide, the catalyst, and at least one solvent.

20. A device comprising the composition of claim 1 .

Assignments (4)
CONFIRMATORY LICENSE Recorded Dec 13, 2021
From: UNIVERSITY OF CALIF-LAWRENC BERKELEY LAB
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 058373/0757 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 20, 2016
From: MICKELSON, WILLIAM; ZETTL, ALEX
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 038661/0147 →
CONFIRMATORY LICENSE Recorded Nov 5, 2015
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 036967/0111 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 31, 2015
From: WORSLEY, MARCUS A.; WOO, LETA YAR-LI
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 036462/0081 →
Continuity (1)
Related Publication 20170036915A1 · Feb 9, 2017