IP Library Granted Patent US 12,410,554
Granted Patent B2
US 12,410,554 · App. 17/617,192 · Granted Sep 9, 2025

System and method of accelerating polymer fiber stabilization via irradiation treatment

Inventors: Xiaodong Li (Charlottesville, VA); Zan Gao (Willimantic, CT); Jiadeng Zhu (Charlottesville, VA); Yellapu V. Murty (Charlottesville, VA); Kenneth Brown (Charlottesville, VA); Clifton Bumgardner (Charlottesville, VA)
Assignee: University of Virginia Patent Foundation
D06M10/001D01F9/22D10B2101/12
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Quick Facts
Patent No.
US 12,410,554
App. No.
17/617,192
Granted
Sep 9, 2025
Kind
B2
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.

Claims (97)

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 said pre-cursor polymeric fibers, tows, yarns, or films.

32. The method of claim 31 , 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.

33. The method of claim 31 , 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.

34. The method of claim 33 , wherein said secondary thermochemical process may comprise: carbonization or microwave-assisted plasma carbonization of said pre-cursor polymeric fibers, tows, yarns, or films.

35. The method of claim 34 , 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.

36. The method of claim 35 , 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.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 18, 2025
From: LI, XIAODONG; GAO, ZAN; ZHU, JIADENG; MURTY, YELLAPU V.; BROWN, KENNETH; BUMGARDNER, CLIFTON
To: UNIVERSITY OF VIRGINIA
Reel/Frame 072048/0982 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 18, 2025
From: UNIVERSITY OF VIRGINIA
To: UNIVERSITY OF VIRGINIA PATENT FOUNDATION
Reel/Frame 072049/0120 →
CONFIRMATORY LICENSE Recorded Jul 11, 2023
From: UNIVERSITY OF VIRGINIA
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 064359/0007 →
Continuity (2)
Provisional Application 62859746 · Jun 11, 2019
Related Publication 20220235516A1 · Jul 28, 2022
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