Methods of growing carbon nanotubes and forming a carbon nanotube thread

Patent metadata

Field	Value
Publication number	US-9796121-B2
Application number	US-201314396962-A
Country	US
Kind code	B2
Filing date	Apr 26, 2013
Priority date	Apr 26, 2012
Publication date	Oct 24, 2017
Grant date	Oct 24, 2017

Abstract

A method of forming an array of aligned, uniform-length carbon nanotubes on a planar surface of a substrate employing a composite catalyst layer of iron and cobalt. The carbon nanotubes have visible length and are useful for producing spun threads of carbon nanotubes having improved spinability and mechanical and electrical properties.

First claim

We claim:

1. A method of forming an array of aligned, uniform-length carbon nanotubes (CNTs) on a planar surface of a substrate, comprising:
1) providing a substrate having a planar surface;
2) depositing a composite catalyst layer on the planar surface, the composite catalyst layer comprising iron and cobalt in an iron to cobalt weight percent ratio of from 20/80 to 50/50;
3) oxidizing the composite catalyst layer to form an oxidized composite catalyst layer;
4) reducing the oxidized composite catalyst layer to form a reduced composite catalyst layer; and
5) growing the array of aligned CNTs on the reduced composite catalyst layer.

2. The method according to claim 1 wherein the composite catalyst layer has a thickness of at least 0.5 nm, and up to 5 nm.

3. The method according to claim 2 wherein the thickness is between 1 nm and 2 nm.

4. The method according to claim 1 wherein forming comprises forming the carbon nanotubes in a chemical vapor deposition reactor.

5. The method according to claim 1 wherein depositing comprises depositing iron and cobalt onto the planar surface simultaneously, or as a plurality of alternating layers of iron and cobalt onto the planar surface.

6. The method according to claim 1 wherein the composite catalyst layer comprises at least approximately 5 wt. % of iron, and up to about 95 wt. % of iron.

7. The method according to claim 1 wherein the deposited composite catalyst layer is a discontinuous layer having a pattern comprising a plurality of coated areas separated by approximately 0.01 mm to approximately 3 mm in distance by an uncoated area.

8. The method according to claim 1 wherein during oxidizing the composite catalyst layer is heated to an annealing temperature of between 300° C. and 900° C.

9. The method according to claim 1 wherein the substrate comprises a layered structure comprising the successive layers of silicon, silicon dioxide, and aluminum oxide, and optionally includes a plurality of the planar surfaces.

10. A method of forming a carbon nanotube CNT thread comprising a plurality of CNTs, comprising:
1) growing an array of aligned CNTs on a planar surface of a substrate, comprising:
i) providing a substrate having a planar surface;
ii) depositing a composite catalyst layer on the planar surface, the composite catalyst layer comprising iron and cobalt in an iron to cobalt weight percent ratio of from 20/80 to 50/50;
iii) oxidizing the composite catalyst layer to form an oxidized composite catalyst layer;
iv) reducing the oxidized composite catalyst layer to form a reduced composite catalyst layer; and
v) growing the array of aligned CNTs on the reduced composite catalyst layer;

2) drawing a plurality of the grown, aligned CNTs from the array of aligned CNTs into a ribbon of CNTs along an axis line; and
3) spinning the ribbon of CNTs about the axis line to form a CNT thread.

11. The method according to claim 7 wherein the coated areas are about 1 mm in diameter.

12. The method according to claim 8 wherein during reducing the oxidized composite catalyst layer is heated to between 600° C. and 800° C. in a reducing gas.

13. The method according to claim 1 wherein the iron to cobalt weight percent ratio is 20/80.

14. The method according to claim 1 wherein the iron to cobalt weight percent ratio is 50/50.

15. The method according to claim 10 wherein the iron to cobalt weight percent ratio is 20/80.

16. The method according to claim 10 wherein the iron to cobalt weight percent ratio is 50/50.

17. The method according to claim 1 wherein the aligned CNTs are predominantly double-walled CNTs.

18. The method according to claim 1 wherein depositing a composite catalyst layer includes depositing an alloy of catalytic elements including iron and cobalt.

Assignees

• Univ Cincinnati

Inventors

• Shanov Vesselin N
• Schulz Mark J

Classifications

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J35/395

  Thickness of the active catalytic layer · CPC title

• C01B2202/08

  Aligned nanotubes · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• D01F9/12

  Carbon filaments; Apparatus specially adapted for the manufacture thereof · CPC title