Carbon nanotubes grown on nanostructured flake substrates and methods for production thereof

Patent metadata

Field	Value
Publication number	US-9963781-B2
Application number	US-26056108-A
Country	US
Kind code	B2
Filing date	Oct 29, 2008
Priority date	Oct 29, 2007
Publication date	May 8, 2018
Grant date	May 8, 2018

Abstract

Carbon nanotubes grown on nanostructured flake substrates are disclosed. The nanostructured flake substrates include a catalyst support layer and at least one catalyst layer. Carbon nanotubes grown on the nanostructured flake substrates can have very high aspect ratios. Further, the carbon nanotubes can be aligned on the nanostructured flake substrates. Through routine optimization, the nanostructured flake substrates may be used to produce single-wall, double-wall, or multi-wall carbon nanotubes of various lengths and diameters. The nanostructured flake substrates produce very high yields of carbon nanotubes per unit weight of substrate. Methods for making the nanostructured flake substrates and for using the nanostructured flake substrates in carbon nanotube synthesis are disclosed.

First claim

What is claimed is:

1. A method for producing substantially aligned, separated carbon nanotubes, wherein the method comprises:
coating a catalyst layer having a thickness of about 0.4 to 2 nm on a support layer comprising Al 2 O 3 on a flexible substrate, said support layer having a thickness of 10 nm to 80 nm;
wherein the coating step comprises electron-beam deposition of the catalyst layer in a high-vacuum roll-to-roll thin film deposition system;
flexing said flexible substrate to release said support layer from said flexible substrate without the use of a solvent so as to form nanostructured, catalyst-coated, flake substrates having diameters of about 2 to 8 μm;
vibrating said nanostructured, catalyst-coated, flake substrates with a piezoelectric oscillator causing the nanostructured, catalyst-coated, flake substrates to become airborne in argon and move through a feed-line to a reactor;
diffusing said nanostructure, catalyst-coated, flake substrates through a coiled tungsten filament in said reactor;
floating said nanostructured, catalyst-coated, flake substrates in a flow of gas of atomic hydrogen and a carbonaceous gas;
growing predominantly separated filaments of substantially aligned single wall carbon nanotubes of greater than 50 μm to 400 μm in length at pressures of 1.4 torr to 15 torr on said nanostructured, catalyst-coated, flake substrates as said nanostructured, catalyst-coated, flake substrates are diffused in a collection area and said nanostructured, catalyst-coated, flake substrates are retained in said collection area by mesh, wherein the growing proceeds at a rate of between about 3 μm per minute and about 20 μm per minute; and
separating the single wall carbon nanotubes from the nanostructured, catalyst-coated, flake substrates by etching the support layer in a KOH bath and etching the catalyst layer from the single wall carbon nanotubes in an acid bath.

2. The method of claim 1 , wherein the catalyst layer comprises Fe.

3. The method of claim 2 , wherein the catalyst layer further comprises at least one additional metal chosen from the group consisting of Mo, Ni, Cr, Co, Pd, Cu and Au.

4. The method of claim 2 , wherein the catalyst is reduced to metallic Fe upon exposure to atomic hydrogen.

5. The method of claim 1 , wherein a length of the substantially aligned carbon nanotubes is controlled by a duration of reaction time.

6. The method of claim 1 , wherein the pressure is 1.4 torr.

7. The method of claim 1 , wherein the carbonaceous gas is acetylene.

8. The method of claim 1 , wherein the floating is performed in a mixture of C 2 H 2 :H 2 O:H 2 at a respective flow rates of 2:2:400 cm 3 /min.

9. The method of claim 1 , wherein the catalyst layer has a thickness of 0.5 nm.

10. The method of claim 1 , further separating the single wall carbon nanotubes from the nanostructured, catalyst-coated, flake substrates by sonication.

Assignees

• Schmidt Howard K
• Hauge Robert H
• Pint Cary L
• Pheasant Sean T
• Coulter Kent E
• Southwest Res Inst
• Univ Rice William M

Inventors

• Schmidt Howard K
• Hauge Robert H
• Pint Cary L
• Pheasant Sean T
• Coulter Kent E

Classifications

• C01B2202/08

  Aligned nanotubes · CPC title

• C01B2202/04

  Nanotubes with a specific amount of walls · CPC title

• C01B2202/36

  Diameter · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01B2202/02

  Single-walled nanotubes · CPC title