Process and apparatus for the production of nanofibers

• US 6,520,425 B1
• Filed: 08/21/2001
• Issued: 02/18/2003
• Est. Priority Date: 08/21/2001
• Status: Expired due to Term

• Current Assignee: University of Akron
• Original Assignee: University of Akron
• Inventors: Reneker, Darrell H.
• Primary Examiner(s): Mar, Michael
• Assistant Examiner(s): Nguyen, Dinh Q.
• Application Number:
  US09/934,228
• Time in Patent Office: 546 Days
• Field of Search: 239/294, 239/290, 239/291, 239/421, 239/423, 239/424.5, 239/425, 239/428, 239/416, 239/416.5, 239/135, 239/137, 239/708, 264/12
• US Class Current: 239/294
• CPC Class Codes: B05B 7/061 with several liquid outlets discharging one or several liquids
• CPC Class Codes: B05B 7/065 an inner gas outlet being surrounded by an annular adjacent liquid outlet
• CPC Class Codes: B05B 7/067 the liquid outlet being annular
• CPC Class Codes: D01D 4/025 Melt-blowing or solution-blowing dies
• CPC Class Codes: D01D 5/00 Formation of filaments, threads, or the like
• CPC Class Codes: D01D 5/0985 by means of a flowing gas (e.g. melt-blowing)
• CPC Class Codes: D04H 1/56 in association with fibre formation, e.g. immediately following extrusion of staple fibres

Abstract

A nozzle for forming nanofibers by using a pressurized gas stream comprises a center tube, a first supply tube that is positioned concentrically around and apart from the center tube, a middle gas tube positioned concentrically around and apart from the first supply tube, and a second supply rube positioned concentrically around and apart from the middle gas tube. The center tube and first supply tube form a first annular column. The middle gas tube and the first supply tube form a second annular column. The middle gas tube and second supply tube form a third annular column. The tubes are positioned so that first and second gas jet spaces are created between the lower ends of the center tube and first supply tube, and the middle gas tube and second supply tube, respectively. A method for forming nanofibers from a single nozzle is also disclosed.

Claims

1. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream comprising:

a center gas tube;

a first fiber-forming material supply tube that is positioned concentrically around and apart from said center gas tube, wherein said center tube and said first fiber-forming material supply tube form a first annular column, and wherein said center gas tube is positioned within said first fiber-forming material supply tube so that a first gas jet space is created between a lower end of said center gas tube and a lower end of said first fiber forming material supply-tube;

a middle gas tube positioned concentrically around and apart from said first supply tube, forming a second annular column;

a second-fiber forming material supply tube positioned concentrically around and apart from said middle gas tube, wherein said middle gas tube and second fiber-forming material supply tube form a third annular column, and wherein said middle gas tube is positioned within said second fiber-forming material supply tube so that a second gas jet space is created between a lower end of said middle gas tube and a lower end of said second fiber-forming material supply tube.

2. A nozzle for forming a plurality of nanofibers according to claim 1, wherein at least one of the first and second gas jet spaces are adjustable.

3. A nozzle for forming a plurality of nanofibers according to claim 1, wherein at least one of the first and second gas jet spaces has a length of about 0.1 to about 10 millimeters.

4. A nozzle for forming a plurality of nanofibers according to claim 1, wherein said center gas tube and said middle gas tube are adapted to carry a pressurized gas at a pressure of from about 10 to about 5000 pounds per square inch.

5. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 4, wherein said pressurized gas is selected from the group consisting of nitrogen, helium, argon, air, carbon dioxide, steam fluorocarbons, fluorochlorocarbons, and mixtures thereof.

6. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 1, further comprising an outer gas tube having an inlet orifice and an outlet orifice, wherein the outer gas tube is positioned concentrically around said second fiber-forming material supply tube, thereby creating an outer gas annular column.

7. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 6, wherein said outer gas tube has a lower end which is on an identical horizontal plane as said lower end of the second fiber-forming material supply tube.

8. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 6, wherein said outer gas tube has a lower end which is on a different horizontal plane than said lower end of the second fiber-forming material supply tube.

9. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 6, wherein at least one of said center gas tube, said middle gas tube and said outer gas tube is adapted to carry a pressurized gas at a pressure of from about 10 to about 5,000 pounds per square inch.

10. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 6, further comprising a gas shroud tube having an inlet orifice and an outlet orifice, wherein said gas shroud tube is positioned concentrically around said outer gas tube.

11. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 10, wherein said gas shroud tube is adapted to carry a gas at a lower pressure and higher flow rate than a gas being supplied though the center gas tube.

12. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 11, wherein said outlet orifice is partially closed by a shroud partition directed radially inward from said gas shroud tube.

13. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 1, wherein said center gas tube and said first fiber-forming material supply tube are essentially parallel to each other.

14. A nozzle for forming a plurality of nanofibers by using a pressurized gas stream according to claim 1, comprising:

means for contacting one or more fiber-forming materials with a plurality of gas streams within said nozzle, such that a plurality of strands of fiber-forming material are ejected from said nozzle, whereupon said strands of fiber-forming material solidify and form nanofibers having a diameter up to about 3000 nanometers.

15. A method for forming a plurality of nanofibers from a single nozzle comprising the steps of:

(A) providing a nozzle containing;

a center tube;

a first supply tube that is positioned concentrically around and apart from said center tube, wherein said center tube and said first supply tube form a first annular column, and wherein said center tube is positioned within said first supply tube so that a first gas jet space is created between a lower end of said center tube and a lower end of said supply tube;

a middle gas tube positioned concentrically around and apart from said first supply tube, forming a second annular column; and

a second supply tube positioned concentrically around and apart from said middle gas tube, wherein said middle gas tube and second supply tube form a third annular column, and wherein said middle gas tube is positioned within said second supply tube so that a second gas jet space is created between a lower end of said middle gas tube and a lower end of said second supply tube; and

(B) feeding one or more fiber-forming materials into said first and second supply tubes;

(C) directing the fiber-forming materials into said first and second gas jet spaces, thereby forming an annular film of fiber-forming material in said first and second gas jet spaces, each annular film having an inner circumference;

(D) simultaneously forcing gas through said center tube and said middle gas tube, and into said first and second gas jet spaces, thereby causing the gas to contact the inner circumference of said annular films in said first and second gas jet spaces, and ejecting the fiber-forming material from the exit orifices of said first and third annular columns in the form of a plurality of strands of fiber-forming material that solidify and form nanofibers having a diameter up to about 3,000 nanometers.

16. The method for forming a plurality of nanofibers from a single nozzle according to claim 15, wherein the nozzle additionally contains an outer gas tube having an inlet orifice and outlet orifice, said outer gas tube being positioned concentrically around and apart from an outermost supply tube, and wherein the method further comprises the step of feeding a cleaner gas through said outer gas column, where the cleaner gas exits the outer gas column at a cleaner orifice that is positioned proximate to an exit orifice of the outermost supply tube, wherein the exit of the cleaner gas thereby prevents the build-up of residual amounts of fiber-forming material at the exit orifice of the outermost supply tube.

17. The method for forming a plurality of nanofibers from a single nozzle according to claim 16, wherein the nozzle additionally contains a shroud gas tube positioned concentrically around and apart from said outer gas tube, said shroud gas tube having an inlet orifice and an outlet orifice, and wherein the method further comprises the step of feeding a shroud gas into said shroud gas tube, such that shroud gas exits the shroud gas tube from the shroud gas tube exit orifice, the exit of the shroud gas thereby influencing the solidification rate of the fiber-forming material being ejected from the exit orifices of the supply tubes.

18. The method for forming a plurality of nanofibers from a single nozzle according to claim 15, further comprising the step of directing the plurality of strands of fiber-forming material exiting from the nozzle into an electric field.