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

• US 7,563,426 B2
• Filed: 12/29/2004
• Issued: 07/21/2009
• 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 C.
• Application Number:
  US11/025,717
• Publication Number:
  US 20060008406A1
• Time in Patent Office: 1,665 Days
• Field of Search: 423/445.B, 423/460, 423/461, 423/DIG.12, 423/447.1, 423/447.3, 110/235, 110/237, 110/243, 977/844, 977/842
• US Class Current: 423/445.00R
• 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. An apparatus including:

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

(b) an injection arrangement for injecting a stream of feed material into the reactant liquid vessel at a point below the reactant liquid level;

(c) a collection chamber positioned to receive effluent escaping from the reactant liquid in the reactant liquid vessel in an effluent ejection area, the collection chamber having a vertical extent defined between a top wall and the surface of the reactant liquid in the effluent ejection area, and having a lateral extent defined between lateral walls extending transverse to the surface of the reactant liquid in the effluent ejection area, the top wall extending transverse to the lateral walls;

(d) a collection surface forming a surface in the collection chamber, the collection surface residing at a position above the reactant liquid level and adjacent to the effluent ejection area; and

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

2. The apparatus of claim 1 wherein the collection surface includes a portion extending in a plane transverse to a device vertical axis.

3. The apparatus of claim 1 further including a reaction chamber portion of the reactant liquid vessel, the reaction chamber portion including an upper wall located below the reactant liquid level in the reactant liquid vessel.

4. The apparatus of claim 1 wherein the collection surface includes graphite.

5. The apparatus of claim 1 further including a water injector conduit extending into the collection chamber.

6. The apparatus of claim 1 further including at least one heating element positioned to apply heat to the volume defined by the collection chamber.

7. A method including:

(a) producing a collection atmosphere in a collection area above a reactant liquid, the collection area having a vertical extent defined between a top wall and the surface of the reactant liquid, and having a lateral extent defined between lateral walls extending transverse to the surface of the reactant liquid, the top wall extending transverse to the lateral walls;

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

(c) maintaining the molecules of the carbon-bearing compound and any reaction products in contact with the reactant liquid for a period of time sufficient to liberate carbon atoms from the molecules of the carbon-bearing compound or reaction products and place the liberated carbon atoms in an excited state;

(d) enabling the liberated carbon atoms in the excited state to traverse a surface of the reactant liquid and flow along a collection path through the collection area so that the liberated carbon atoms pass over a collection surface in the collection area, the collection surface comprising a surface distinct from the lateral walls and the top wall; and

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

8. The method of claim 7 wherein the heat is applied to the collection area from at least one of the lateral walls or from the top wall.

9. The method of claim 7 further including adding water vapor to the collection area while the liberated carbon atoms pass over the collection surface.

10. An apparatus including:

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

(b) an injection arrangement for injecting a stream of feed material into the reactant liquid vessel at a point below the reactant liquid level;

(c) a collection chamber positioned to receive effluent escaping from the reactant liquid in the reactant liquid vessel in an effluent ejection area, the collection chamber having a vertical extent defined between a top wall and the surface of the reactant liquid in the effluent ejection area, and having a lateral extent defined between lateral walls extending transverse to the surface of the reactant liquid in the effluent ejection area, the top wall extending transverse to the lateral walls;

(d) a collection surface forming a surface in the collection chamber, the collection surface residing at a position above the reactant liquid level and adjacent to the effluent ejection area, and being distinct from the lateral walls and top wall; and

(e) at least one 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 between the reactant liquid and the collection surface.

11. The apparatus of claim 10 wherein at least one heating element is positioned in at least one of the lateral walls.

12. The apparatus of claim 10 wherein at least one heating element is positioned in the top wall.

13. The apparatus of claim 10 wherein at least one heating element is positioned in a structure forming the collection surface.

14. The apparatus of claim 10 further including a collection surface charging device operatively connected to the collection surface to produce a desired electrical charge on the collection surface.

15. A method including:

(a) producing a collection atmosphere in a collection area above a reactant liquid, the collection area having a vertical extent defined between a top wall and the surface of the reactant liquid, and having a lateral extent defined between lateral walls extending transverse to the surface of the reactant liquid, the top wall extending transverse to the lateral walls;

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

(c) maintaining the molecules of the carbon-bearing compound and any reaction products in contact with the reactant liquid for a period of time sufficient to liberate carbon atoms from the molecules of the carbon-bearing compound or reaction products and place the liberated carbon atoms in an excited state;

(d) enabling the liberated carbon atoms in the excited state to traverse a surface of the reactant liquid and flow along a collection path through the collection area so that the liberated carbon atoms pass over a collection surface in the collection area, the collection surface comprising a surface distinct from the lateral walls and the top wall; and

(e) applying an electrical charge to the collection surface in the collection area as liberated carbon atoms in the excited state flow along the collection path.

16. The method of claim 15 further including heating the collection area from a heating element located above the surface of the reactant liquid.

17. The method of claim 16 wherein at least one heating element is positioned in at least one of the lateral walls.

18. The method of claim 16 wherein at least one heating element is positioned in the top wall.

19. The method of claim 16 wherein at least one heating element is positioned in a structure forming the collection surface.