Method and apparatus for preparing a collection area for use in producing carbon nanostructures

• US 7,814,846 B2
• Filed: 10/31/2007
• Issued: 10/19/2010
• Est. Priority Date: 07/09/2004
• Status: Expired due to Fees

• Current Assignee: Clean Technology International Corp.
• Original Assignee: Clean Technology International Corp.
• Inventors: Wagner, Anthony S.
• Primary Examiner(s): Hendrickson; Stuart L.
• Assistant Examiner(s): MCCRACKEN, DANIEL
• Application Number:
  US11/932,020
• Publication Number:
  US 20100172817A1
• Time in Patent Office: 1,084 Days
• Field of Search: 423/445.B, 423/460, 423/461, 423/DIG.12, 423/447.1, 423/447.2, 423/447.3, 110/235, 110/237, 110/243, 977/842, 977/844
• US Class Current: 110/235
• CPC Class Codes: B01J 19/24 Stationary reactors without moving elements inside B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02
• CPC Class Codes: B01J 19/26 Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• CPC Class Codes: B01J 21/185 Carbon nanotubes carbon nanotubes per se C01B32/15
• CPC Class Codes: B01J 2219/00119 Heat exchange inside a feeding nozzle or nozzle reactor
• CPC Class Codes: B01J 2219/00135 Electric resistance heaters
• CPC Class Codes: B01J 2219/00182 controlling the level of reactants in the reactor vessel
• CPC Class Codes: B01J 23/10 of rare earths
• CPC Class Codes: B01J 23/24 Chromium, molybdenum or tungsten
• CPC Class Codes: B01J 23/38 of noble metals
• CPC Class Codes: B01J 23/70 of the iron group metals or copper
• CPC Class Codes: B01J 37/023 using molten compounds
• CPC Class Codes: B01J 4/002 Nozzle-type elements nozzle-type reactors B01J19/26
• CPC Class Codes: B01J 6/005 Fusing
• 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 32/162 characterised by catalysts
• CPC Class Codes: C01B 32/90 Carbides
• CPC Class Codes: Y10S 977/842 for carbon nanotubes or fullerenes
• CPC Class Codes: Y10S 977/844 Growth by vaporization or dissociation of carbon source using a high-energy heat source, e.g. electric arc, laser, plasma, e-beam

Abstract

A method includes producing deposition conditions in a collection area above a reactant liquid containing one or more catalyst metals. The reactant liquid is maintained under conditions in which atoms of the catalyst metal may escape from the reactant liquid into the collection area. A suitable carrier gas is directed to traverse a surface of the reactant liquid and flow along a collection path that passes over a collection surface in the collection area. This flow of carrier gas is maintained so that escaped atoms of catalyst metal are entrained in the gas traversing the surface of the reactant liquid and are deposited on the collection surface prior to or concurrently with nanocarbon structure formation at the collection surface.

Claims

1. A method including:

(a) purging a collection area of oxygen, the collection area comprising an area defined immediately above a surface of a reactant liquid;

(b) injecting a feed material into the reactant liquid, the feed material including a quantity of a carbon-bearing compound;

(c) reacting the carbon-bearing compound in the reactant liquid to liberate carbon atoms and place the liberated carbon atoms in an excited state;

(d) enabling the liberated carbon atoms in the excited state to traverse the surface of the reactant liquid and flow into the collection area; and

(e) heating the collection area from a heating element located above the surface of the reactant liquid.

2. The method of claim 1 wherein the collection area is defined in part between lateral walls extending transverse to the surface of the reactant liquid and wherein the heat is applied to the collection area from at least one of the lateral walls.

3. The method of claim 1 wherein the collection area is defined between lateral walls extending transverse to the surface of the reactant liquid and between the surface of the reactant liquid and a top wall and wherein the heat is applied to the collection area from the top wall.

4. The method of claim 1 further including adding water vapor to the collection area while the liberated carbon atoms traverse the surface of the reactant liquid and pass into the collection area.

5. The method of claim 1 wherein the collection area is defined in part between lateral walls extending transverse to the surface of the reactant liquid and further including:

(a) providing a collection surface within the collection area, the collection surface being separate from the lateral walls; and

(b) producing a desired electrical charge on the collection surface.

6. The method of claim 1 further including providing a collection surface within the collection area and wherein the collection surface includes graphite.

7. The method of claim 1 further including providing a collection surface within the collection area and wherein the collection surface includes one or more catalyst metals.

8. The method of claim 7 wherein at least one of the catalyst metals on the collection surface is deposited from the reactant liquid.

9. An apparatus including:

(a) a reactant liquid vessel for containing a reactant liquid at a reactant liquid level;

(b) an injection conduit having an end positioned to release a feed material into the reactant liquid vessel at a point below the reactant liquid level;

(c) a collection chamber positioned immediately above a surface of the reactant liquid to receive effluent escaping from the reactant liquid in the reactant liquid vessel in an effluent ejection area; and

(d) a heating element located above the reactant liquid level in position to apply heat to maintain a desired temperature in the volume defined by the collection chamber immediately above the reactant liquid level.

10. The apparatus of claim 9 wherein the collection chamber is defined in part by lateral walls extending transverse to the reactant liquid level and further including a collection surface forming a surface in the collection chamber, the collection surface residing at a position above the reactant liquid level and being distinct from the lateral walls.

11. The apparatus of claim 9 wherein the collection chamber is defined in part by lateral walls extending transverse to the reactant liquid level and wherein the heating element is positioned in at least one of the lateral walls.

12. The apparatus of claim 9 wherein the collection chamber is defined in part by a top wall spaced apart from the reactant liquid level and wherein the heating element is positioned in the top wall.

13. The apparatus of claim 9 further including a collection surface formed in the collection chamber, the collection surface being distinct from lateral walls and a top wall which define the collection chamber, and wherein the heating element is positioned in a structure forming the collection surface.

14. The apparatus of claim 9 further including at least one additional heating element located above the reactant liquid level in position to apply heat to the volume defined by the collection chamber.

15. The apparatus of claim 9 further including:

(a) a collection surface formed in the collection chamber, the collection surface being distinct from lateral walls and a top wall which define the collection chamber; and

(b) a collection surface charging device operatively connected to the collection surface to produce a desired electrical charge on the collection surface.

16. A method including:

(a) producing a collection atmosphere in a collection area, the collection area comprising an area defined immediately above a surface of a reactant liquid;

(b) injecting a feed material into the reactant liquid, the feed material including a quantity of a carbon-bearing compound;

(c) reacting molecules of the carbon-bearing compound in the liquid reactant to liberate carbon atoms and place the liberated carbon atoms in an excited state;

(d) enabling the liberated carbon atoms in the excited state to traverse the surface of the reactant liquid and flow into the collection area; and

(e) heating the collection area from a heating element located above the surface of the reactant liquid.

17. The method of claim 16 wherein the collection area is defined in part between lateral walls extending transverse to the surface of the reactant liquid and wherein the heat is applied to the collection area from at least one of the lateral walls.

18. The method of claim 16 wherein the collection area is defined between lateral walls extending transverse to the surface of the reactant liquid and between the surface of the reactant liquid and a top wall and wherein the heat is applied to the collection area from the top wall.

19. The method of claim 16 wherein the collection area is defined in part between lateral walls extending transverse to the surface of the reactant liquid and further including providing a collection surface within the collection area, the collection surface being separate from the lateral walls.

20. The method of claim 19 further including producing a desired electrical charge on the collection surface.