IP Library Granted Patent US 11,643,735
Granted Patent B2
US 11,643,735 · App. 16/414,503 · Granted May 9, 2023

Methods and systems for production of elongated carbon nanofibers

Inventor: Stuart Licht (Venice, FL)
Assignee: C2CNT LLC
C25B1/00B01J23/755B01J23/8926B01J23/8993C01B32/16C01B32/162C25B1/135C25D9/02C25D9/08D01F9/12B82Y30/00B82Y40/00C01B2202/34
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Quick Facts
Patent No.
US 11,643,735
App. No.
16/414,503
Granted
May 9, 2023
Kind
B2
Abstract

A system and process for producing macro length carbon nanotubes is disclosed. A carbonate electrolyte including transition metal powder is provided between a nickel alloy anode and a nickel alloy cathode contained in a cell. The carbonate electrolyte is heated to a molten state. An electrical current is applied to the nickel alloy anode, nickel alloy cathode, and the molten carbonate electrolyte disposed between the anode and cathode. The resulting carbon nanotube growth is collected from the cathode of the cell.

Claims (52)

1. A method for producing elongated macroscopic carbon nanotubes comprising:

heating a carbonate electrolyte to obtain a molten carbonate electrolyte;

disposing the molten carbonate electrolyte between an anode and a cathode in a cell;

applying an electrical current to the cathode and the anode in the cell; and

collecting carbon nanotube growth from the cathode of the cell,

wherein the method includes

(a) the molten carbonate electrolyte consists essentially of a transition metal powder;

(b) the cathode comprises copper, a nickel copper alloy, a nickel chromium alloy, or a brass alloy, and

(c) the anode comprises a nickel chromium alloy, a nickel copper alloy, or a nickel iron alloy.

2. The method of claim 1 , wherein said alloy of the anode is a nickel copper alloy and contains 10% nickel to 90% nickel and 10% copper to 90% copper.

3. The method of claim 1 , wherein said alloy of the anode is a nickel chromium alloy and contains 10% nickel to 90% nickel and 10% chromium to 90% chromium.

4. The method of claim 1 , wherein said alloy of the anode is a nickel iron alloy and contains 10% nickel to 90% nickel and 10% iron to 90% iron.

5. The method of claim 1 , wherein the molten carbonate electrolyte has a melting point between about 150° C. and about 900° C.

6. The method of claim 1 , wherein the molten carbonate electrolyte consists essentially of lithium carbonate.

7. The method of claim 1 , wherein the molten carbonate electrolyte consists essentially of at least one material selected from the group consisting of: lithium carbonate; sodium carbonate; potassium carbonate; strontium carbonate; rubidium carbonate; cesium carbonate; barium carbonate; and calcium carbonate, and any combination thereof.

8. The method of claim 1 , wherein the produced carbon nanotubes are longer than 1 mm in length.

9. The method of claim 1 , wherein the carbon nanotubes are a cluster of untangled carbon nanotubes.

10. The method of claim 1 , wherein the carbon nanotubes are a cluster of tangled carbon nanotubes.

11. The method of claim 1 , further comprising cleaning the carbon nanotubes with a solvent.

12. The method of claim 1 , further comprising separating carbon nanotubes from the carbon nanotube growth.

13. The method of claim 1 , further comprising separating carbon nanotube cotton from the carbon nanotube growth.

14. The method of claim 13 , further comprising spinning spun fiber from the carbon nanotube cotton.

15. The method of claim 1 , further comprising fabricating a composite material comprising carbon nanotubes collected from the carbon nanotubes.

16. The method of claim 15 , wherein the composite material is a carbon cloth.

17. The method of claim 15 , wherein the composite material is a carbon cable.

18. The method of claim 15 , wherein the composite material is a carbon wire.

19. The method of claim 1 , further comprising aging the molten carbonate electrolyte for a predetermined amount of time prior to applying the electrical current.

20. The method of claim 1 , wherein the anode further comprises at least one material selected from the group consisting of: manganese; titanium; zirconium; molybdenum; tantalum; cobalt; silicon; carbon, and any combination thereof.

21. The method of claim 1 , wherein the anode further comprises at least two materials selected from the group consisting of: manganese; titanium; zirconium; molybdenum; tantalum; cobalt; silicon; carbon, and any combination thereof.

22. The method of claim 1 , wherein the cathode does not have a zinc coating.

23. The method of claim 22 , wherein the transition metal powder is selected from nickel, chromium, iron, cobalt, manganese, titanium, zirconium, copper, vanadium, zinc, molybdenum, scandium, ruthenium, tantalum, and alloys thereof.

24. The method of claim 1 , wherein the method is conducted at an electrolysis temperature of between 700° C. and 900° C.

25. A method for producing a macro length carbon nanotube comprising:

providing a carbonate electrolyte including transition metal powder between a nickel alloy anode and a nickel alloy cathode contained in a cell;

heating the carbonate electrolyte to a molten state;

applying an electrical current to the nickel alloy anode, nickel alloy cathode, and the molten carbonate electrolyte disposed between the anode and cathode; and

collecting carbon nanotube growth from the cathode of the cell.

26. The method of claim 25 , wherein the nickel alloy of the anode is a nickel copper alloy and contains 10% nickel to 90% nickel and 10% copper to 90% copper.

27. The method of claim 25 , wherein the nickel alloy of the anode is a nickel chromium alloy and contains 10% nickel to 90% nickel and 10% chromium to 90% chromium.

28. The method of claim 25 , wherein the nickel alloy of the anode is a nickel iron alloy and contains 10% nickel to 90% nickel and 10% iron to 90% iron.

29. The method of claim 25 , wherein the transition metal powder includes particles of at least one material selected from the group consisting of: nickel; chromium; iron; cobalt; manganese; titanium; zirconium; copper; vanadium; zinc; molybdenum; scandium; ruthenium; tantalum; and alloys and mixtures thereof.

30. The method of claim 25 , wherein the transition metal powder includes particles of at least two materials selected from the group consisting of: nickel; chromium; iron; cobalt; manganese; titanium; zirconium; copper; vanadium; zinc; molybdenum; scandium; ruthenium; tantalum; and alloys and mixtures thereof.

31. The method of claim 25 , wherein said transition metal powder has a diameter of 10 μm or larger.

32. The method of claim 25 , wherein said transition metal powder has a diameter of 1 to 10 μm.

33. The method of claim 25 , wherein said transition metal particle has a diameter of less than 1 μm.

34. A method for producing elongated carbon nanotubes comprising:

(i) applying an electrical current to a cathode and an anode which are disposed in a molten carbonate electrolyte, where the molten carbonate electrolyte consists essentially of a transition metal powder, to form carbon nanotubes having a length of at least 0.4 mm, where

(a) the cathode comprises copper, a nickel copper alloy, a nickel chromium alloy, or a brass alloy, and

(b) the anode comprises a nickel chromium alloy, a nickel copper alloy, or a nickel iron alloy; and

(ii) collecting carbon nanotube growth from the cathode of the cell.

35. The method of claim 34 , wherein the carbon nanotubes are longer than 1 mm in length.

36. The method of claim 34 , wherein the transition metal powder is selected from nickel, chromium, cobalt, manganese, titanium, zirconium, copper, vanadium, zinc, molybdenum, scandium, ruthenium, tantalum, and alloys thereof.

Assignments (2)
REDOMICILE IN FLORIDA Recorded Nov 5, 2022
From: C2CNT LLC
To: C2CNT LLC
Reel/Frame 061884/0781 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 31, 2021
From: LICHT, STUART
To: C2CNT LLC
Reel/Frame 055777/0333 →
Continuity (3)
Continuation PCTUS2017061861 · Nov 15, 2017
Provisional Application 62423052 · Nov 16, 2016
Related Publication 20190271088A1 · Sep 5, 2019