IP Library Granted Patent US 8,367,034
Granted Patent B2
US 8,367,034 · App. 11/628,256 · Granted Feb 5, 2013

Methods for preparing single-walled carbon nanotubes

Inventors: Stephen O'Brien (New York, NY); Limin Huang (New York, NY); Brian Edward White (Walton, NY)
Assignee: The Trustees of Columbia University in the City of New York
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Quick Facts
Patent No.
US 8,367,034
App. No.
11/628,256
Granted
Feb 5, 2013
Kind
B2
Abstract

The present invention relates to cobalt and molybdenum doped mesoporous silica catalysts and methods for using the catalysts to making Single-Walled Carbon Nanotubes. The methods offer increased control over the orientation, length and diameter of the nanotubes produced.

Claims (30)

1. A method for making a single-walled carbon nanotube, the method comprising:

affixing a catalyst precursor solution to a surface of a substrate, wherein the catalyst precursor solution comprises mesoporous silica, cobalt, and molybdenum, wherein the affixing the catalyst precursor solution comprises at least one of spin-coating, dip-coating, drop-coating, contact printing, or micro-patterning the catalyst precursor solution onto the surface of the substrate;

heating the substrate, for a time and temperature sufficient to calcine the catalyst precursor solution to form a calcined catalyst; and

contacting the calcined catalyst with a flow of carbon feedstock gas for a time and at a temperature sufficient to make a single-walled carbon nanotube.

2. The method of claim 1 , wherein the substrate comprises one of a silica wafer, a silicate, a flake, a silicon wafer, or a silicon wafer having an oxide layer.

3. The method of claim 1 , wherein the mesoporous silica comprises at least one of SBA16, SBA15, SBA11, MCM41, or MCM48.

4. The method of claim 1 , wherein the catalyst precursor solution is affixed to the substrate surface using at least one of spin-coating, dip-coating, or drop-coating.

5. The method of claim 1 , wherein the catalyst precursor solution is affixed to the substrate surface using contact printing.

6. The method of claim 5 , wherein the catalyst precursor solution is affixed to the substrate surface as a micro-pattern.

7. The method of claim 1 , comprising growing the nanotube in a direction parallel to the flow of carbon feedstock gas.

8. The method of claim 1 , wherein the nanotube has a diameter of from about 0.3 nm to about 4 nm.

9. The method of claim 8 , wherein the nanotube has a diameter of from about 0.5 nm to about 3 nm.

10. The method of claim 9 , wherein the nanotube has a diameter of from about 0.8 nm to about 1.8 nm.

11. The method of claim 1 , wherein the nanotube has a length of from about 1 nm to about 100 cm.

12. The method of claim 11 , wherein the nanotube has a length of from about 1 mm to about 10 cm.

13. The method of claim 11 , wherein the nanotube has a length of from about 100 mm to about 1 cm.

14. The method of claim 1 , wherein the nanotube is an individual nanotube.

15. The method of claim 1 , wherein the substrate is heated for about 2 hours at a temperature of about 550° C.

16. The method of claim 1 , wherein heating the substrate is carried out at a temperature of from about 350° C. to about 1000° C.

17. The method of claim 16 , wherein the temperature is from about 700° C. to about 850° C.

18. The method of claim 17 , wherein the temperature is about 850° C.

19. The method of claim 1 , wherein the carbon feedstock comprises ethanol.

20. The method of claim 1 , wherein the carbon feedstock is mixed with argon gas.

21. The method of claim 1 , wherein the flow rate of the carbon feedstock gas is between about 20 sccm to about 1000 sccm.

22. The method of claim 21 , wherein the flow rate of the carbon feedstock gas is between about 20 sccm to about 100 sccm.

23. The method of claim 21 , wherein the flow rate of the carbon feedstock gas is between about 500 sccm to about 800 sccm.

24. The method of claim 1 , wherein the surface of the substrate has one or more slits.

25. The method of claim 1 , wherein the surface of the substrate has one or more trenches.

26. The method of claim 15 , wherein the heating is performed in air.

27. The method of claim 1 , comprising preparing the catalyst precursor solution by preparing a mesoporous silica solution and incorporating cobalt and molybdenum into the mesoporous silica solution.

Assignments (3)
CONFIRMATORY LICENSE Recorded May 14, 2014
From: COLUMBIA UNIVERSITY
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 032913/0812 →
CONFIRMATORY LICENSE Recorded Dec 29, 2010
From: COLUMBIA UNIVERSITY NEW YORK MORNINGSIDE
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 025571/0015 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 24, 2007
From: O'BRIEN, STEPHEN; HUANG, LIMIN; WHITE, BRIAN EDWARD
To: THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK
Reel/Frame 019870/0341 →
Continuity (2)
Provisional Application 60577110 · Jun 4, 2004
Related Publication 20080069760A1 · Mar 20, 2008