Method for manufacturing carbon nanotubes

Patent metadata

Field	Value
Publication number	US-9394625-B2
Application number	US-201414224085-A
Country	US
Kind code	B2
Filing date	Mar 25, 2014
Priority date	Sep 14, 2007
Publication date	Jul 19, 2016
Grant date	Jul 19, 2016

Abstract

A method for manufacturing carbon nanotubes is provided. First, a substrate having a first surface and a second surface opposite to the first surface is provided. Second, a catalyst film is formed on the first surface of the substrate, wherein the catalyst film comprises a carbonaceous material. Third, a mixture of a carrier gas and a carbon source gas is flew across the catalyst film. Forth, a focused laser beam is irradiated on the substrate to grow a carbon nanotube array from the substrate.

First claim

What is claimed is:

1. A method for manufacturing carbon nanotubes comprising:
providing an apparatus comprising:
an observation device comprising an observation tube, an observation window arranged on the top of the observation tube, a first half-reflecting pellicle mirror installed at an angle of 45° in the observation tube, and a second half-reflecting pellicle mirror installed parallel to the first half-reflecting pellicle mirror;
a work stage disposed under and separated a certain distance from the observation tube;
a laser device arranged perpendicular to the observation device and optically directed at the first half-reflecting pellicle mirror;
a lighting device arranged perpendicular to the observation device and optically directed at the second half-reflecting pellicle mirror;

providing a substrate have a first surface and a second surface opposite to the first surface;
forming a catalyst film on the first surface of the substrate, wherein the catalyst film comprises a carbonaceous material;
flowing a mixture of a carrier gas and a carbon source gas across the catalyst film; and
irradiating a focused laser beam on the substrate to grow a carbon nanotube array from the substrate, wherein the catalyst film is configured to grow carbon nanotubes by heating the substrate locally, and the observation device is configured to observe the carbon nanotubes during the growth process.

2. The method of claim 1 , wherein the forming the catalyst film on the first surface of the substrate comprises:
providing a mixture of a dispersant and a carbonaceous material;
mixing the mixture with a solvent to form a solution;
ultrasonically agitating the solution to promote dispersing the carbonaceous material therein;
adding a soluble catalyst material into the dispersed solution to form a catalyst solution;
coating the catalyst solution on the first surface of the substrate; and
baking the substrate to form the catalyst film thereon.

3. The method of claim 2 , wherein the dispersant is sodium dodecyl benzene sulfonate, and a weight ratio of the dispersant to the carbonaceous material is in a range from about 1:2 to about 1:10.

4. The method of claim 2 , wherein the catalyst solution comprises about 0.01 to about 0.5 Mol/L magnesium nitrate and about 0.01 to about 0.5 Mol/L iron nitrate.

5. The method of claim 2 , wherein the soluble catalyst material comprises one or more metallic nitrate compounds selected from the group consisting of magnesium nitrate (Mg(NO 3 ) 2 .6H 2 O), iron nitrate (Fe(NO 3 ) 3 .9H 2 O), cobalt nitrate (Co(NO 3 ) 2 .6H 2 O), nickel nitrate (Ni(NO 3 ) 2 .6H 2 O), and any combination thereof.

6. The method of claim 2 , wherein the substrate with the catalyst solution coated thereon is baked at about 60 to about 100° C. for several tens of minutes.

7. The method of claim 2 , wherein the carbonaceous material comprises a material selected from the group consisting of carbon black, graphite, and any combination thereof.

8. The method of claim 1 , wherein the catalyst film comprises a material selected from the group consisting of iron, gallium nitride, cobalt, nickel, and any combination alloy thereof.

9. A method for manufacturing carbon nanotubes comprising:
providing an apparatus comprising:
an observation device comprising an observation tube, an observation window arranged on the top of the observation tube, a first half-reflecting pellicle mirror installed at an angle of 45° in the observation tube, and a second half-reflecting pellicle mirror installed parallel to the first half-reflecting pellicle mirror;
a work stage disposed under and separated a certain distance from the observation tube;
a laser device arranged perpendicular to the observation device and optically directed at the first half-reflecting pellicle mirror;
a lighting device arranged perpendicular to the observation device and optically directed at the second half-reflecting pellicle mirror;

providing a substrate having a first surface and a second surface opposite to the first surface;
forming a light absorption film on the first surface of the substrate;
forming a catalyst film on the light absorption film, wherein the catalyst film comprises a first carbonaceous material;
flowing a mixture of a carrier gas and a carbon source gas across the catalyst film; and
irradiating a focused laser beam on the substrate to grow a carbon nanotube array from the substrate, wherein the catalyst film is configured to grow carbon nanotubes by heating the substrate locally, and the observation device is configured to observe the carbon nanotubes during the growth process.

10. The method of claim 9 , wherein forming the light absorption film on the first surface of the substrate comprises:
applying a second carbonaceous material layer onto the first surface of the substrate;
gradually heating the substrate with the second carbonaceous material layer to about 300 to about 450° C. for about 60 to about 90 minutes in an atmosphere of N 2 and/or another inert gas and baking the substrate with the second carbonaceous material thereon for about 15 to about 20 minutes; and
cooling down the substrate with the second carbonaceous material thereon to room temperature, thereby forming the light absorption layer on the first surface of the substrate.

11. The method of claim 10 , wherein the second carbonaceous material layer is a colloidal graphite inner coating (GIC) layer.

12. The method of claim 11 , wherein a thickness of the formed light absorption film is in a range from about 1 micrometer to about 20 micrometers.

13. The method of claim 11 , wherein forming the catalyst film on the light absorption film comprises:
providing a catalyst-ethanol solution; and
coating the catalyst-ethanol solution on the GIC layer to form the film of catalyst thereon.

14. The method of claim 13 , wherein the catalyst-ethanol solution is a mixture solution of ethanol and one or more metallic nitrate compounds selected from the group consisting of magnesium nitrate (Mg(NO 3 ) 2 .6H 2 O), iron nitrate (Fe(NO 3 ) 3 .9H 2 O), cobalt nitrate (Co(NO 3 ) 2 .6H 2 O), nickel nitrate (Ni(NO 3 ) 2 .6H 2 O), and any combination thereof.

15. The method of claim 13 , wherein the catalyst-ethanol solution comprises about 0.01 to about 0.5 Mol/L magnesium nitrate and about 0.01 to about 0.5 Mol/L iron nitrate.

Assignees

• Univ Tsinghua
• Hon Hai Prec Ind Co Ltd

Inventors

• Luo Chun-Xiang
• Jiang Kai-Li
• Fan Shou-Shan

Classifications

• C30B25/16

  Controlling or regulating (controlling or regulating in general G05) · CPC title

• C01B31/0206

  Chemistry & Metallurgy · mapped topic

• C30B29/605

  Products containing multiple oriented crystallites, e.g. columnar crystallites · CPC title

• C01B31/0226

  Chemistry & Metallurgy · mapped topic

• B82Y30/00 Primary

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