CVD method of producing and doping fullerenes

• US 5,510,098 A
• Filed: 01/03/1994
• Issued: 04/23/1996
• Est. Priority Date: 01/03/1994
• Status: Expired due to Fees

• Current Assignee: University of Central Florida (State University System of Florida)
• Original Assignee: University of Central Florida (State University System of Florida)
• Inventors: Chow, Lee
• Primary Examiner(s): Lewis, Michael
• Assistant Examiner(s): DI MAURO, PETER T
• Application Number:
  US08/176,543
• Time in Patent Office: 841 Days
• Field of Search: 423/446, 423/445 B, 423/262, 423/263, 423/439
• US Class Current: 423/445.00B
• 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 32/15 Nano-sized carbon materials
• CPC Class Codes: C01B 32/152 Fullerenes
• CPC Class Codes: C01B 32/154 Preparation
• CPC Class Codes: C01B 32/156 After-treatment
• CPC Class Codes: Y10S 977/843 Gas phase catalytic growth, i.e. chemical vapor deposition

Abstract

Methods of producing fullerenes in large-macroscopic quantities inexpensively is disclosed without using solid carbon material such as graphite. In a preferred embodiment, fullerenes are formed by a hot filament CVD procedure. The fullerenes occur in the soot that forms as a by-product on the edges of the substrate holder. Mass spectrum of soot deposits shows lines corresponding to C₆₀. From the typical concentrations of gaseous species in the diamond-growing CVD chamber, hydrocarbon species including CH₃ or C₂ H₂ can be the precursors for the formation of fullerenes in the CVD chamber. A method of using fullerenes to enhance the properties of rubber composites is also described.

Claims

1. A method of producing fullerenes using an electrically heated metal filament to deposit soot containing fullerenes on a substrate within a Chemical Vapor Deposition chamber, comprising the steps of:

(a) feeding and mixing, under fullerene growth conditions to increase the yield of fullerenes-containing soot, approximately 0.5 to 2% CH₄ gas with approximately 98 to 99.5% H₂ gas into a Chemical Vapor Deposition chamber containing a substrate and a metal filament;

(b) raising the temperature of the metal filament in the chamber to approximately 2200 degrees C.;

(c) maintaining the temperature of the substrate to be between approximately 900 to 950 degrees C.;

(d) collecting soot from the substrate in the chamber; and

(e) extracting fullerenes from the collected soot.

2. The method of producing fullerenes of claim 1, wherein the filament is approximately 0.5 to 1.0 mm tungsten wire.

3. The method of producing fullerenes of claim 1, wherein the providing step further includes

maintaining current between approximately 30 to 100 A to the filament.

4. The method of producing fullerenes of claim 1, further including the step of:

evacuating the chamber.

5. The method of producing fullerenes of claim 4, wherein the chamber is evacuated between:

approximately 30 to approximately 60 torr.

6. The method of producing fullerenes of claim 1, wherein the step of maintaining includes:

moving the substrate relative to the filament.

7. The method of producing fullerenes of claim 1, wherein the step of removing further includes:

removing soot from a substrate holder in the chamber.

8. The method of producing fullerenes of claim 1, wherein the step of feeding further includes:

adding at least one additive gas chosen from at least one of;

He, Ne, Ar, La, Ni, Na, Rb, and Cs.

9. A method of producing fullerenes using an electrically heated metal filament and a substrate within a Chemical Vapor Deposition chamber, comprising the steps of:

(a) providing a current maintained at approximately 30 to 100 A to a tungsten filament within a Chemical Vapor Deposition chamber;

(b) feeding and mixing, under fullerene growth conditions to increase the yield of fullerenes-containing soot, approximately 0.5 to 2% CH₄ gas and approximately 98 to 99.5% H₂ gas to the chamber;

(c) maintaining the temperature of a silicon substrate in the chamber to be approximately 900 to 950 degrees C.;

(d) collecting soot from the substrate in the chamber; and

(e) extracting fullerenes from the collected soot.

10. The method of producing fullerenes of claim 9, wherein the tungsten filament is approximately 0.5 to 1.0 mm wire.

11. The method of producing fullerenes of claim 9, further including the step of:

evacuating the chamber.

12. The method of producing fullerenes of claim 11, wherein the chamber is evacuated between:

approximately 30 to approximately 60 torr.

13. The method of producing fullerenes of claim 9, wherein the step of maintaining further includes:

moving the substrate relative to the filament to adjust the temperature of the filament.

14. The method of producing fullerenes of claim 9, wherein the step of removing further includes:

removing soot from a substrate holder in the chamber.

15. The method of producing fullerenes of claim 9, wherein the step of feeding further includes:

adding additive gases chosen from at least one of;

He, Ne, Ar, La, Ni, Na, Rb, and Cs.