Atmospheric pressure plasma processing of polymeric materials utilizing close proximity indirect exposure

Patent metadata

Field	Value
Publication number	US-9447205-B2
Application number	US-201213680406-A
Country	US
Kind code	B2
Filing date	Nov 19, 2012
Priority date	Nov 19, 2012
Publication date	Sep 20, 2016
Grant date	Sep 20, 2016

Abstract

A plasma treatment method that includes providing treatment chamber including an intermediate heating volume and an interior treatment volume. The interior treatment volume contains an electrode assembly for generating a plasma and the intermediate heating volume heats the interior treatment volume. A work piece is traversed through the treatment chamber. A process gas is introduced to the interior treatment volume of the treatment chamber. A plasma is formed with the electrode assembly from the process gas, wherein a reactive species of the plasma is accelerated towards the fiber tow by flow vortices produced in the interior treatment volume by the electrode assembly.

First claim

What is claimed is:

1. A method for plasma stabilization and oxidation of a polymeric workpiece, the method comprising:
providing a treatment chamber including an intermediate heating volume and an interior treatment volume, wherein the interior treatment volume contains an electrode assembly for generating a plasma and the intermediate heating volume heats the interior treatment volume; traversing said polymeric workpiece through the interior treatment volume, provided that said polymeric workpiece is in an indirect close proximity of 1 to 30 cm from said electrode assembly, and said polymeric workpiece is comprised of a polymeric material; introducing an oxygen-containing process gas to the interior treatment volume of the treatment chamber; and
forming the plasma with the electrode assembly from the oxygen-containing process gas in said interior treatment volume, wherein a reactive species of the plasma is accelerated towards the polymeric workpiece by flow vortices produced in the interior treatment volume, wherein said flow vortices result from an asymmetrical electric field gradient produced by an asymmetrical electrode geometry, and wherein said plasma stabilization and oxidation results in at least oxidation and crosslinking of the polymeric workpiece through the interior region of the polymeric workpiece.

2. The method of claim 1 , wherein the intermediate heating volume increases a. temperature of the interior treatment volume up to 500° C.

3. The method of claim 1 , wherein the electrode assembly comprises at least one first electrode on a first side of a dielectric surface and at least one second electrode on an opposing second dielectric surface.

4. The method of claim 1 , wherein the polymeric workpiece comprises a fiber tow.

5. The method of claim 1 , wherein a treated portion of the polymeric workpiece is present in the interior treatment volume for a time period ranging from 1 minute to 300 minutes.

6. The method of claim 1 , wherein the oxygen-containing process gas that is introduced to the interior treatment volume comprises a gas selected from the group consisting of air, oxygen, nitrogen oxides, carbon dioxide, carbon monoxide, oxygen-containing gas, and combinations thereof.

7. The method of claim 1 , wherein the process gas is a gas mixture of nitrogen (N 2 ) and diatomic molecular oxygen (O 2 ), wherein, the diatomic molecular oxygen (O 2 ) content may range from 10% to 100% and the nitrogen (N 2 ) content may range from 0% to 95%.

8. The method of claim 1 , wherein the forming of the plasma comprises applying an alternating current (AC) to the electrode assembly in a frequency range of 30 Hz to 20 MHz.

9. The method of claim 1 , wherein the reactive species of the plasma is selected from the group consisting of O 2 , O x ,O, N x O y ,H x O y , and ions, radicals, excited states and metabolic stables of the process gas.

10. The method of claim 1 , wherein the polymeric workpiece is comprised of polyacrylonitrile (PAN) and the reactive species is comprised of an oxygen containing species, wherein the reactive species oxidizes the polymeric workpiece.

11. The method of claim 1 , wherein the electrode assembly for generating the plasma includes a plurality of plasma forming electrode assemblies, which can be independently energized to provide a temperature gradient along a length of the interior treatment volume.

12. The method of claim 1 , wherein said polymeric workpiece is in a close proximity of 1 to 20 cm from said electrode assembly.

13. The method of claim 1 , wherein said polymeric workpiece is in a close proximity of 1 to 15 cm from said electrode assembly.

14. The method of claim 1 , wherein said intermediate heating volume is an exterior heating volume that surrounds said interior treatment volume, wherein the exterior heating volume is defined by an outer shell and an inner shell and heats the interior treatment volume, wherein the inner shell separates the exterior heating volume from the interior treatment volume and defines the volume and shape of the interior treatment volume.

15. The method of claim 1 , wherein said polymeric material is selected from the group consisting of rayon, polyacrylonitrile (PAN), petroleum, coal-based pitch, lignin, and combinations thereof.

16. The method of claim 1 , wherein said plasma is operated at a pressure of 1 torr to 1500 torr.

17. The method of claim 1 , wherein said plasma is operated at a pressure of 250 torr to 800 torr.

18. The method of claim 1 , wherein said plasma is operated at a pressure of approximately 760 torr.

Assignees

• Ut Battelle Llc
• Remaxco Tech

Inventors

• Paulauskas Felix L
• Bonds Truman

Classifications

• D06B19/00

  Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00 · CPC title

• B01J2219/0879

  Solid · CPC title

• H01J37/32522

  Temperature · CPC title

• B01J2219/0871

  Heating or cooling of the reactor · CPC title

• D01F9/22

  from polyacrylonitriles · CPC title