IP Library Granted Patent US 11,434,574
Granted Patent B2
US 11,434,574 · App. 17/243,510 · Granted Sep 6, 2022

System, method and composition for making thin-walled carbon nanomaterials

Inventor: Stuart Licht (Venice, FL)
Assignee: C2CNT LLC
C25B1/135C25B11/046B82Y40/00
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Quick Facts
Patent No.
US 11,434,574
App. No.
17/243,510
Granted
Sep 6, 2022
Kind
B2
Abstract

The present disclosure relates to thin-walled carbon nanomaterial, such as thin-walled carbon nanotubes, and systems, methods and compositions for production thereof. The method for producing a thin walled carbon nanotube comprises 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, limiting a diameter of the carbon nanomaterial.

Claims (47)

1. A system for making a thin-walled carbon nanomaterial product (CNM), the system comprising:

a. an anode;

b. a cathode;

c. an inter-electrode space that is defined between the anode and the cathode;

d. a carbonate electrolyte media positionable within the inter-electrode space,

e. a source of current for applying a current density is at least 0.01 A/cm 2 across the electrodes;

f. a source of heat configured to heat the electrolyte media to a temperature so as to create a molten electrolyte media;

g. a diameter-limiting component that is mixable with the electrolyte media, wherein the diameter-limiting component is configured to provide an oxidative and/or conductive environment within the inter-electrode space, and wherein the diameter-limiting component comprises calcium metaborate, boric acid combined with calcium oxide, or a combination thereof; and

h. a source of carbon for introducing a carbon input into the inter-electrode space.

2. The system of claim 1 , wherein the diameter-limiting component is calcium metaborate.

3. The system of claim 1 , wherein the diameter-limiting component is a combination of boric acid and calcium oxide.

4. The system of claim 1 , wherein the diameter-limiting component is present in amount of about 0.01 to about 5 molal with respect to the carbonate electrolyte media or the molten carbonate electrolyte media.

5. The system of claim 1 , wherein the anode and cathode are positioned substantially parallel to each other and aligned substantially vertically within the system.

6. The system of claim 5 , wherein the anode is a Nichrome sheet that is about 0.01 to 1 inch thick and the cathode is a brass sheet that is about 0.01 to 1 inch thick.

7. The system of claim 6 , wherein the anode is two series connected anodes and the cathode is positioned therebetween separated for each anode by about 0.1 to about 4 inches.

8. The method of claim 7 , wherein the step of limiting the diameter of the CNM comprises mixing the diameter-limiting component with the molten carbonate electrolyte media.

9. The method of claim 7 , wherein the diameter-limiting component is calcium metaborate.

10. The method of claim 7 , wherein the diameter-limiting component comprises a combination of boric acid and calcium oxide.

11. The system of claim 1 , wherein the source of carbon is carbon dioxide.

12. A method for producing a thin-walled carbon nanomaterial (CNM), the method comprising:

a. heating a carbonate electrolyte media to obtain a molten carbonate electrolyte contained within a cell;

b. disposing the molten carbonate electrolyte between an anode and a cathode;

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

d. limiting a diameter of the thin-walled CNM by mixing a diameter-limiting component with the electrolyte media or the molten carbonate electrolyte, wherein the diameter-limiting component comprises calcium metaborate, boric acid combined with calcium oxide, or a combination thereof, wherein the step of limiting the diameter of the thin-walled CNM comprises:

i. adding about 0.01 to about 5 molal of a diameter-limiting component comprising calcium metaborate, boric acid combined with calcium oxide, lithium oxide, or a combination thereof to the carbonate electrolyte media or to the molten carbonate electrolyte media;

ii. modulating the electrical current to a low electrolysis current density;

iii. providing an oxidative environment within the inter-electrode space;

iv. providing a conductive environment within the inter-electrode space; or

v. any combination thereof.

13. The method of claim 12 , further comprising a step of selecting a nanomaterial morphology.

14. The method of claim 12 , wherein the step of limiting the diameter of the CNM comprises mixing the diameter-limiting component with the carbonate electrolyte media.

15. The method of claim 12 , wherein the diameter-limiting component is added in amount of about 0.01 to about 5 molal with respect to the carbonate electrolyte media or the molten carbonate electrolyte media.

16. The method of claim 12 , wherein the step of limiting the diameter of the CNM produced comprises modulating the electrical current to a low electrolysis current density.

17. The method of claim 12 , wherein the step of limiting the diameter of the CNM produced further comprises a step of stopping the electrical current between about 5 minutes and about 90 minutes.

18. The method of claim 12 , further comprising a step of collecting the thin-walled carbon nanomaterial product from the cathode.

19. The method of claim 12 , wherein the electrolysis current is alternating current.

20. The method of claim 19 , further comprising a step of adding zinc oxide to the cell.

21. An electrolyte media for making a thin-walled carbon nanomaterial product, the electrolyte media comprising:

a. a carbonate; and

b. a diameter-limiting component, wherein the diameter-limiting component is configured to provide an oxidative and/or conductive environment for making the thin-walled carbon nanomaterial product, and wherein the diameter-limiting component comprises calcium metaborate, boric acid combined with calcium oxide, or a combination thereof.

22. The electrolyte media of claim 21 , wherein the carbonate is an alkali carbonate, an alkali earth carbonate or combinations thereof.

23. The electrolyte media of claim 22 , wherein the electrolyte media further comprises an oxide, a borate, a sulfate, a nitrate, a chloride, a chlorate, a phosphate or combinations thereof.

24. The electrolyte media of claim 21 , wherein the diameter-limiting component is calcium metaborate, boric acid combined with calcium oxide, or a combination thereof.

25. The electrolyte media of claim 21 , wherein the diameter-limiting component is present in an amount of about 0.01 to about 5 molal with respect to the carbonate.

26. The electrolyte media of claim 21 in a molten state.

27. The electrolyte media of claim 21 , wherein the diameter-limiting component is calcium metaborate.

28. The electrolyte media of claim 21 , wherein the diameter-limiting component comprises a combination of boric acid and calcium oxide.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 15, 2021
From: LICHT, STUART
To: C2CNT LLC
Reel/Frame 058115/0946 →
Continuity (2)
Provisional Application 63017489 · Apr 29, 2020
Related Publication 20210340680A1 · Nov 4, 2021