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

Patent metadata

Field	Value
Publication number	US-11434574-B2
Application number	US-202117243510-A
Country	US
Kind code	B2
Filing date	Apr 28, 2021
Priority date	Apr 29, 2020
Publication date	Sep 6, 2022
Grant date	Sep 6, 2022

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.

First claim

What is claimed is:

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.

Assignees

• C2Cnt Llc

Inventors

• Licht Stuart

Classifications

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• C01B2202/36

  Diameter · CPC title

• C01B32/16 Primary

  Preparation · CPC title

• C25B11/046

  Alloys · CPC title

• C25B1/135 Primary

  Carbon · CPC title