Method for obtaining carbon nanotubes on supports and composites comprising same

• US 20070189953A1
• Filed: 01/21/2005
• Published: 08/16/2007
• Est. Priority Date: 01/30/2004
• Status: Abandoned Application

• Current Assignee: Centre National De La Recherche Scientifique
• Original Assignee: Centre National De La Recherche Scientifique
• Inventors: Ci, Li-Jie, Bai, Jinbo, Zhao, Zhig-Gang
• Application Number:
  US10/587,546
• Publication Number:
  US 20070189953A1
• Time in Patent Office: Days
• US Class Current: 423/414
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 2202/06 Multi-walled nanotubes
• CPC Class Codes: C01B 2202/36 Diameter
• CPC Class Codes: C01B 32/162 characterised by catalysts
• CPC Class Codes: C23C 16/26 Deposition of carbon only

Abstract

The invention concerns a method for obtaining carbon nanotubes by CVD growth on nano/micrometric supports, characterized in that it comprises: adding a carbon source compound containing a catalyst, under an inert gas and hydrogen current. The invention is applicable to the manufacture of multiple-scale composites.

Claims

1. A process for obtaining carbon nanotubes by growth, using the CVD method, on nanoscale/microscale supports, characterized in that it comprises:

the addition of a compound as carbon source containing a catalyst, into a stream of inert gas and hydrogen.

2. The process as claimed in claim 1, characterized in that it also gcomprises:

the heating, in a reaction chamber, of a nanoscale/microscale ceramic material or of carbon fibers, to a temperature of 600-1100°

C., in a stream of inert gas;

the cooling of the chamber down to room temperature; and

the recovery of the product formed.

3. The process as claimed in claim 2, characterized in that the ceramic material is in the form of nanoscale/microscale particles or fibers.

4. The process as claimed in claim 3, characterized in that the ceramic material is formed from the following:

carbon fibers;

glass fibers;

SiC, TiC, Al₂O₃, SiO₂ or B₄C particles and fibers;

silica fume;

clays (clay particles);

or wires comprising a metallic material such as Fe, Ni, Co, Ti, Pt, Au, Y, Ru, Rh, Pd, Zr, Cr or Mn.

5. The process as claimed in claim 1, characterized in that the compound as carbon source is chosen from the following:

liquid hydrocarbons of the group comprising xylene, toluene and benzene;

or n-pentane;

or alcohols, such as ethanol and methanol;

or ketones, such as acetone;

or, as a variant, the compound as carbon source is a gaseous hydrocarbon such as acetylene, methane, butane, propylene, ethylene and propene;

or the compound as carbon source is solid, such as for example camphor.

6. The process as claimed in claim 1, characterized in that the catalyst is chosen from the group comprising the following:

an iron, cobalt or nickel metallocene;

or else iron, cobalt or nickel nitrates, acetates or sulfates, especially Fe(II), phthalocyanine (FePc) and iron pentacarbonyl (Fe(CO)₅).

7. The process as claimed in claim 1, characterized in that the catalyst and the compound as carbon source are used in an amount from 0.001 to 0.1 g of catalyst per ml of compound.

8. The process as claimed in claim 1, characterized in that the ratio of inert gas to hydrogen is 5/95 to 50/50.

9. The process as claimed in claim 1, characterized in that, before said step of heating the support material, a silicon-containing compound is used under conditions allowing silicon or a silicon derivative, such as SiC, SiO or SiO₂, to be deposited on the surface of the support material.

10. The process as claimed in claim 9, characterized in that the silicon-containing compound used is SiO or a silane, such as SiCl₄.

11. Products thus obtained by the process as claimed in claim 1, characterized in that they are multiscale composites formed from carbon nanotubes bonded to nanoscale/microscale carbon fiber or ceramic fiber support materials.

12. Multiscale composites, characterized in that they comprise carbon nanotubes bonded to nanoscale/microscale supports in a polymer, metal or ceramic matrix.