System and method of accelerating polymer fiber stabilization via irradiation treatment

Patent metadata

Field	Value
Publication number	US-12410554-B2
Application number	US-202017617192-A
Country	US
Kind code	B2
Filing date	Jun 10, 2020
Priority date	Jun 11, 2019
Publication date	Sep 9, 2025
Grant date	Sep 9, 2025

Abstract

A new technique for treating non-PAN-based pre-cursor polymeric fibers, tows, yarns, and films has been created for use in making stabilized pre-cursor polymers. By applying stepwise or non-stepwise microwave and/or ultraviolet radiation to the pre-cursor polymeric fibers, tows, yarn, or films prior to the stabilization thereof, a reduction in time for the costly stabilization process is achieved. Application of this technique extends to less-costly production of carbon fibers, for uses in industries such as automotive, aviation, trains, medical, military, sporting goods, orthopedics, and other industries. The pre-cursor polymeric fibers, tows, yarns, or films may be a multi-component polymer composite comprised of a non-PAN-based polymeric fiber, tow, yarn, or film and at least one or more constituent materials. Carbonization of such pre-cursor polymeric fibers, tows, yarns, or films results in less-costly carbon fibers that perform equally, if not better, than traditional costly PAN-based carbon fibers.

First claim

What is claimed is:

1. A method for treating pre-cursor polymeric fibers, tows, yarns, or films, said method comprising:
irradiating the pre-cursor polymeric fibers, tows, yarns, or films with specified duration exposure to microwaves and/or ultraviolet light;
cooling the irradiated pre-cursor polymeric fibers, tows, yarns, or films;
wherein said pre-cursor polymeric fiber, tow, yarn, or film is a multi-component polymer composite comprised of a polymeric fiber, tow, yarn, or film and at least one or more constituent materials;
wherein the polymeric fiber, tow, yarn, or film comprises polyamide; and
wherein the at least one or more constituent materials comprises one of the following metallic compounds: CuCl, CuCl 2 , or FeCl 3 .

2. The method of claim 1 , wherein the specified duration of the irradiation has the duration of one of the following ranges:
about 5 seconds to about 60 seconds;
about 60 seconds to about 10 minutes;
about 10 minutes to about 20 minutes;
about 20 minutes to about 30 minutes;
about 30 minutes to about 45 minutes; or
about 45 minutes to about 60 minutes.

3. The method of claim 1 , wherein the irradiation of claim 1 , is applied at one of the following:
a power of a range between about 100W and about 100 kW;
a power of a range between about 100W and about 1000W; or
a power of about 700W.

4. The method of claim 1 , wherein said exposure to microwaves comprises exposure to microwave frequencies in the range of about 300 GHz to about 300 MHz.

5. The method of claim 1 , wherein said exposure to microwaves comprises exposure to microwave frequency of about 2.45 GHz.

6. The method of claim 1 , wherein the polymeric fiber, tow, yarn, or film comprises polyamide, polyethylene, high-density polyethylene (HDPE), ultra-high molecular weight polyethylene (UHMWPE), other bio-sourced polymer, or a non-PAN-based polymer.

7. The method of claim 1 , wherein the at least one or more constituent materials comprise graphene.

8. The method of claim 1 , wherein the treated pre-cursor polymeric fibers, tows, yarns, or films have a diameter in the range of about 5 μm to about 250 μm.

9. The method of claim 1 , wherein the pre-cursor polymeric fiber, tow, yarn, or film is already spun or otherwise prepared prior to the irradiation.

10. The method of claim 1 , wherein said exposure to ultraviolet light comprises exposure to ultraviolet light wavelengths in the range of about 10 nm to about 450 nm.

11. The method of claim 10 , wherein said exposure to ultraviolet light comprises exposure to ultraviolet light wavelength of about 405 nm.

12. The method of claim 1 , wherein said at least one or more constituent materials defines a constituent content having a concentration comprising a range of one of the following:
about 0.01% to about 1%; or
about 0.05% to about 0.1%,
of the multi-component polymer composite.

13. The method of claim 12 , wherein said at least one or more constituent materials comprises the following: graphene, borophene, boron carbide, carbon nanotubes, or other nanomaterials.

14. The method of claim 1 , further comprising heating the cooled irradiated pre-cursor polymeric fibers, tows, yarns, or films to achieve stabilization of said pre-cursor polymeric fibers, tows, yarns, or films.

15. The method of claim 14 , wherein the stabilization is provided over a duration of one of the following ranges:
about 15 hours to about 25 hours;
about 10 hours to about 15 hours;
about 5 hours to about 10 hours;
about 2 hours to about 5 hours; or
about 1 hour to about 2 hours.

16. The method of claim 14 , wherein the heating occurs at a temperature within one of the following ranges:
about 150° C. to about 300° C.;
about 200° C. to about 250° C.;
about 250° C. to about 300° C.; or
about 200° C. to about 215° C.

17. The method of claim 16 , further comprising at least one or more additional heating occurrences to achieve a secondary thermochemical process to said pre-cursor polymeric fibers, tows, yarns, or films.

18. The method of claim 17 , wherein said secondary thermochemical process may comprise: thermal carbonization or microwave-assisted plasma carbonization of said pre-cursor polymeric fibers, tows, yarns, or films.

19. The method of claim 18 , wherein said additional heating includes increasing the heat at a ramp rate in the range of about 0.5° C. to about 25° C. per minute to a final temperature in the ranges of about 1000° C. to about 1700° C. or of about 500° C. to about 3000° C. to achieve the carbonization of said pre-cursor polymeric fibers, tows, yarns, or films.

20. The method of claim 19 , wherein the carbonization occurs over a duration of one of the following:
a range of about 15 minutes to about 3 hours;
a range of about 1 hour to about 2 hours;
a range of about 30 minutes to about 60 minutes; or
about 30 minutes.

21. The method of claim 1 , further comprising:
irradiating the irradiated pre-cursor polymeric fibers, tows, yarns, or films with specified duration exposure to microwaves and/or ultraviolet light; and
cooling the irradiated pre-cursor polymeric fibers, tows, yarns, or films.

22. The method of claim 21 , wherein said specified duration of the irradiation of claim 21 is a longer duration, shorter duration, or equal duration as that of the duration of the irradiation in claim 1 .

23. The method of claim 21 , wherein said specified duration of the irradiation of claim 21 is of one of the following ranges:
about 5 seconds to about 120 minutes;
about 5 seconds to about 60 seconds;
about 60 seconds to about 10 minutes;
about 10 minutes to about 20 minutes;
about 20 minutes to about 30 minutes;
about 30 minutes to about 45 minutes;
about 45 minutes to about 60 minutes; or
about 60 minutes to about 120 minutes.

24. The method of claim 21 , wherein the irradiation of claim 2 , is applied at one of the following:
a power of a range between about 100W and about 100 kW;
a power of a range between about 100W and about 1000W; or
a power of about 700W.

25. The method of claim 21 , wherein the treated pre-cursor polymeric fibers, tows, yarns, or films have a diameter in the range of about 5 μm to about 250 μm.

26. The method of claim 21 , wherein said irradiating and cooling of claim 21 are repeated a specified number of times of one of the following ranges:
between 5 and 10 times; or
between 1 and 4 times.

27. The method of claim 26 , wherein said duration of the irradiation is sequentially longer.

28. The method of claim 26 , wherein the heating occurs at a temperature within one of the following ranges:
about 150° C. to about 300° C.;
about 200° C. to about 250° C.;
about 250° C. to about 300° C.; or
about 200° C. to about 215° C.

29. The method of claim 26 , wherein the irradiation of claim 13 , is applied at one of the following:
a power of a range between about 100W and about 100 kW;
a power of a range between about 100W and about 1000W; or
a power of about 700W.

30. The method of claim 26 , wherein the treated pre-cursor polymeric fibers, tows, yarns, or films have a diameter in the range of about 5 μm to about 250 μm.

31. The method of claim 26 , further comprising heating the cooled irradiated pre-cursor polymeric fibers, tows, yarns, or films to achieve stabilization of

Assignees

• Univ Virginia Patent Foundation

Inventors

• Li Xiaodong
• Gao Zan
• Zhu jiadeng
• Murty Yellapu V
• Brown Kenneth
• Bumgardner Clifton

Classifications

• D10B2101/12

  Carbon; Pitch · CPC title

• D01F9/22

  from polyacrylonitriles · CPC title

• D06M2101/34

  Polyamides · CPC title

• D06M11/28

  Halides of elements of Groups 8, 9, 10 or 18 of the Periodic Table · CPC title

• D06M11/13

  Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table · CPC title