IP Library Granted Patent US 11,440,851
Granted Patent B1
US 11,440,851 · App. 16/275,630 · Granted Sep 13, 2022

Method of making carbon matrix composite from high temperature polymer matrix fiber-reinforced composites

Inventors: Richard D. Hreha (Dayton, OH); Kristopher K. Aber (Dayton, OH); Joel P. Brubaker (Dayton, OH); Kristin M. Cable (Dayton, OH); Michael D. Rauscher (Beavercreek, OH)
Assignee: Systima Technologies, Inc.
C04B35/83C04B35/64C08J5/042C04B2235/422C04B2235/5248C04B2235/658C04B2235/6562C04B2235/6565C04B2235/6567
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Quick Facts
Patent No.
US 11,440,851
App. No.
16/275,630
Granted
Sep 13, 2022
Kind
B1
Abstract

Methods of producing a carbon matrix composite are provided which include preparing a carbon matrix composite precursor comprising at least one carbon-based reinforcement material and a cured thermoset polymer matrix comprising a chemical composition in accordance with Formula I where n and m are integers, at least one of R 1 or R 2 comprises an aromatic moiety, and X is selected from the group consisting of CH 2 , NH, O, S, SO 2 , and combinations thereof. The methods further include heating the carbon matrix composite precursor in air to a first processing temperature of between 300° C. and 500° C. to form a carbon matrix composite intermediate, and heating the carbon matrix composite intermediate in nitrogen to a second processing temperature of between 900° C. to 1650° C. and holding at the second processing temperature for at least 1 hour in an inert gas environment to form the carbon matrix composite.

Claims (34)

1. A method of producing a carbon matrix composite, the method comprising:

preparing a carbon matrix composite precursor, the carbon matrix composite precursor comprising at least one carbon-based reinforcement material and a cured thermoset polymer matrix comprising a chemical composition in accordance with Formula I

wherein:

m and n are each an integer greater than or equal to 1,

at least one of R 1 or R 2 comprises an aromatic moiety, and

X is selected from the group consisting of CH 2 , NH, O, S, SO 2 , and combinations thereof;

heating the carbon matrix composite precursor to a first processing temperature, wherein:

the first processing temperature is between 300° C. and 500° C. to form a carbon matrix composite intermediate, and

the heating to the first processing temperature is completed in an atmosphere comprising air; and

heating the carbon matrix composite intermediate to a second processing temperature and holding at the second processing temperature for at least 1 hour to form the carbon matrix composite, wherein:

the second processing temperature is between 900° C. to 1650° C., and

the heating to the second processing temperature and hold at the second processing temperature is completed in an inert gas environment.

2. The method of claim 1 , wherein the carbon-based reinforcement material comprises carbon fiber.

3. The method of claim 1 , wherein carbon-based reinforcement material comprises carbon fiber, random carbon mats, carbon fiber scrims, chopped carbon fibers, carbon fiber knits, unidirectional carbon fiber plies, three-dimensional carbon fober weaves, three-dimensional carbon fiber preforms, prepreg carbon fiber, plain weave fabric, twill fabrics, or combinations thereof.

4. The method of claim 1 , wherein the method further comprises cooling the carbon matrix composite intermediate to room temperature under the atmosphere comprising air before heating the carbon matrix composite intermediate to the second processing temperature in the inert gas environment.

5. The method of claim 1 , wherein the first processing temperature is between 350° C. and 445° C.

6. The method of claim 1 , wherein the second processing temperature is between 900° C. and 1100° C.

7. The method of claim 1 , wherein the heating the carbon matrix composite precursor to the first processing temperature is completed at a rate of 0.5° C. to 2° C. per minute.

8. The method of claim 1 , wherein the heating the carbon matrix composite intermediate to the second processing temperature is completed at a rate of 0.5° C. to 2° C. per minute.

9. The method of claim 4 , wherein the cooling the carbon matrix composite intermediate to room temperature under the atmosphere comprising air is completed at a rate of 0.5° C. to 2° C. per minute.

10. The method of claim 1 , wherein n, m, or both, are integers from 1 to 200.

11. The method of claim 1 , wherein R 1 , R 2 , or both comprise one or more of a phenyl group, a naphthyl group, a benzyl group, or a 4-cyanophenyl group.

12. The method of claim 1 , wherein R 1 , R 2 , or both comprise one or more of an ether group, a sulfur group, a sulfonyl group, an imine group, an amide group, a methylene group, a dialkyl methylene group, an isopropyl group, a trifluoromethyl group, a hexafluoroisopropyl group, a carbonyl group, a methyl group, a propyl group, a dimethylamino group, or a boronic acid group.

13. The method of claim 1 , wherein R 1 , R 2 , or both comprise one or more of an (1-(5-(1-(5-Formyl-2-furfyl)-1-methylethyl)-2-furfyl)-1-methylethyl), diphenylsulfone, diphenyl sulfone, diphenyl ether, 1,3-bis(phenoxy)-benzene, moiety, 4,4′-(1,3-phenylenedioxy)dianiline, 1,3-bis(3-aminophenoxy)benzene, 4,4′-oxydianiline, 4-aminophenyl sulfone, 3-aminophenyl sulfone, or isophthalaldehyde derivatives.

14. The method of claim 1 , wherein the carbon matrix composite precursor comprises 32 to 42 percent by weight of the carbon-based reinforcement material and 58 to 68 percent by weight of the cured thermoset polymer matrix comprising the chemical composition in accordance with Formula I.

15. The method of claim 1 , wherein the method further comprises at least one densification process, the densification process comprising:

infiltrating the carbon matrix composite with a polymer resin;

curing the polymer resin introduced in the infiltrating step; and

heating the carbon matrix composite with cured polymer resin infiltrated therein to the first processing temperature in an atmosphere comprising air, and subsequently in an inert gas environment to the second processing temperature and holding at the second processing temperature for at least 1 hour in the inert gas environment.

16. The method of claim 15 , wherein the polymer resin comprises the chemical composition in accordance with Formula I, a phenolic resin based polymer, a furan resin based polymer, or combinations thereof.

17. The method of claim 1 , wherein the heating the carbon matrix composite precursor to the first processing temperature is completed at a rate of 0.5° C. to 10° C. per minute.

18. The method of claim 1 , wherein the heating the carbon matrix composite intermediate to the second processing temperature is completed at a rate of 0.5° C. to 10° C. per minute.

19. The method of claim 4 , wherein the cooling the carbon matrix composite intermediate to room temperature under the atmosphere comprising air is completed at a rate of 0.5° C. to 20° C. per minute.

20. The method of claim 1 , wherein the inert gas environment consists of a nitrogen atmosphere.

Assignments (8)
SECURITY INTEREST Recorded Apr 8, 2025
From: SYSTIMA TECHNOLOGIES, INC.
To: CITIBANK, N.A., AS AGENT
Reel/Frame 070775/0023 →
RELEASE OF SECURITY INTEREST Recorded Apr 8, 2025
From: TCW ASSET MANAGEMENT COMPANY, LLC
To: SYSTIMA TECHNOLOGIES, INC.
Reel/Frame 070767/0592 →
SECURITY INTEREST Recorded Sep 30, 2022
From: SYSTIMA TECHNOLOGIES, INC.
To: TCW ASSET MANAGEMENT COMPANY, LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 061276/0116 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 2, 2022
From: CORNERSTONE RESEARCH GROUP, INCORPORATED
To: SYSTIMA TECHNOLOGIES, INC.
Reel/Frame 060694/0679 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 27, 2022
From: CORNERSTONE RESEARCH GROUP, INCORPORATED
To: SYSTIMA TECHNOLOGIES, INC.
Reel/Frame 060318/0876 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 14, 2022
From: JALAPENO HOLDINGS, LLC
To: CORNERSTONE RESEARCH GROUP, INC.
Reel/Frame 059595/0149 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 6, 2019
From: CORNERSTONE RESEARCH GROUP, INC.
To: JALAPENO HOLDINGS, LLC
Reel/Frame 048518/0186 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 6, 2019
From: HREHA, RICHARD D.; ABER, KRISTOPHER K.; BRUBAKER, JOEL P.; CABLE, KRISTIN M.; RAUSCHER, MICHAEL D.
To: CORNERSTONE RESEARCH GROUP, INC.
Reel/Frame 048518/0082 →
Continuity (1)
Provisional Application 62630509 · Feb 14, 2018