IP Library › Granted Patent US 12,129,560
Granted Patent B2
US 12,129,560 · App. 17/858,906 · Granted Oct 29, 2024

Graphene and the production of graphene

Inventors: René Hoffmann (Freiburg, DE); Christoph E. Nebel (Freiburg, DE); Sarah Roscher (Freiburg, DE)
Assignee: Avadain LLC
C25B1/00C01B32/19C01B32/198C25B9/19C25B9/40C25B11/043H01B1/04H01M4/587H01M4/625B82Y30/00B82Y40/00C01B2204/04C01P2002/82C01P2004/03C01P2004/24Y10S977/734Y10S977/842
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Quick Facts
Patent No.
US 12,129,560
App. No.
17/858,906
Granted
Oct 29, 2024
Kind
B2
Abstract

Compositions comprising hydrogenated and dehydrogenated graphite comprising a plurality of flakes. At least one flake in ten has a size in excess of ten square micrometers. For example, the flakes can have an average thickness of 10 atomic layers or less.

Claims (35)

1. A composition comprising:

dehydrogenated graphite comprising a plurality of flakes having

at least one flake in 10 of the plurality of flakes having a size in excess of 10 square micrometers,

an average thickness of 10 atomic layers or less, and

a defect density characteristic of at least 50% of μ-Raman spectra of the dehydrogenated graphite collected at 532 nm excitation with a resolution better than 1.8 reciprocal centimeters having a D/G area ratio below 0.5, wherein the composition is a composite and at least 30% of sp 3 hybridized carbon sites of the composition are

cross-linked with sp 3 hybridized carbon sites of another flake of the plurality of flakes.

2. The composition of claim 1 , wherein more than 60% of μ-Raman spectra of the dehydrogenated graphite have the coefficient of determination value larger than 0.99.

3. The composition of claim 1 , wherein more than 40% of the μ-Raman spectra of the dehydrogenated graphite have the coefficient of determination value larger than 0.995.

4. The composition of claim 1 , wherein at least one flake in six of the plurality of flakes has a size in excess of 10 square micrometers.

5. The composition of claim 1 , wherein at least one flake in ten of the plurality of flakes has a size in excess of 25 square micrometers.

6. The composition of claim 1 , wherein the average thickness is seven atomic layers or less.

7. The composition of claim 1 , wherein the defect density is characteristic of at least 80% of the collected spectra having a D/G area ratio below 0.5.

8. The composition of claim 1 , wherein the defect density is characteristic of at least 50% of the collected spectra having a D/G area ratio below 0.2.

9. The composition of claim 1 , wherein the composition is a particulate powder of dehydrogenated graphite flakes.

10. The composition of claim 1 , wherein the plurality of the flakes are wrinkled, crumpled, or folded.

11. The composition of claim 1 , wherein the full width half maximum of the G peak in μ-Raman spectra of the dehydrogenated graphite collected at 532 nm excitation with a resolution better than 1.8 reciprocal centimeters is larger than 20 reciprocal centimeters.

12. The composition of claim 1 , wherein more than 1% of the plurality of flakes have a thickness of more than 10 atomic layers.

13. The composition of claim 12 , wherein more than 5% of the plurality of flakes have a thickness of more than 10 atomic layers.

14. The composition of claim 13 , wherein more than 10% of the plurality of flakes have a thickness of more than 10 atomic layers.

15. The composition of claim 1 , wherein the flakes of the plurality of flakes have an average surface area of more than 50 square micrometers.

16. The composition of claim 15 , wherein the plurality of flakes have an average surface area of more than 100 square micrometers.

17. A composition comprising:

a reversibly hydrogenated graphite comprising a plurality of flakes having

at least one flake in 10 of the plurality of flakes having a size in excess of 10 square micrometers,

a coefficient of determination value of 2D single peak fitting of μ-Raman spectra of the graphite after thermal treatment in inert atmosphere at 2 mbar and 800° C., collected at 532 nm excitation with a resolution better than 1.8 reciprocal centimeters, of larger than 0.99 for more than 50% of the spectra, and

a defect density characteristic of μ-Raman spectra of the hydrogenated graphite collected at 532 nm excitation with a resolution better than 1.8 reciprocal centimeters and an excitation power below 2 mW at the focus of an 100λ objective having an average D/G area ratio being between 0.2 and 4, wherein the majority of the defects are reversible hydrogenation of sp 3 -hybridized carbon sites away from the edges of the flakes of the plurality of flakes, wherein more than 60% of μ-Raman spectra of the graphite have the coefficient of determination value larger than 0.99, and wherein at least 60% of the defects are reversible hydrogenation of sp 3 -hybridized carbon sites away from the edges of the flakes of the plurality of flakes, and wherein the composition is a composite and at least 5% of sp 3 hybridized carbon sites of the composition are one or more of

a) functionalized with a non-hydrogen chemical group, or

b) cross-linked with sp 3 hybridized carbon sites of another flake of the plurality of flakes.

18. The composition of claim 17 , wherein more than 40% of the μ-Raman spectra of the graphite have the coefficient of determination value larger than 0.995.

19. The composition of claim 17 , wherein at least one flake in ten of the plurality of flakes has a size in excess of 25 square micrometers.

20. The composition of claim 17 , wherein the average thickness is seven atomic layers or less.

21. The composition of claim 17 , wherein the defect density is characteristic of at least 50% of the μ-Raman spectra collected at 532 nm excitation with a resolution better than 1.8 reciprocal centimeters and an excitation power below 2 mW at the focus of an 100λ objective having a D/G area ratio above 0.5.

22. The composition of claim 17 , wherein the defect density is characteristic of at least 50% of the collected spectra having a D/G area ratio above 0.8.

23. The composition of claim 17 , wherein the defect density is characteristic of the average D/G area ratio being between 0.4 and 2.

24. The composition of claim 17 , wherein the composition includes interstitial hydrogen and/or organic solvents or salts between the flakes of the plurality of flakes.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 1, 2022
From: HOFFMANN, RENÉ; NEBEL, CHRISTOPH E.; ROSCHER, SARAH
To: AVADAIN LLC
Reel/Frame 060680/0265 →
Priority Claims (1)
DE 102016202202 · Feb 12, 2016 · national
Continuity (4)
Continuation 16882579 · May 25, 2020
Continuation 15642086 · Jul 5, 2017
Continuation PCTEP2016073451 · Sep 30, 2016
Related Publication 20230002913A1 · Jan 5, 2023