# US 12,006,411 B1 · Method of making carbonized composites

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- Number: US 12,006,411 B1
- Document ID: US12006411B1
- Status: Granted
- Kind: B1
- Application number: 17/405,454
- Filed: 2021-08-18
- Granted: 2024-06-11
- Earliest claimed: 2020-08-19
- Assignees: Systima Technologies, Inc.
- Applicants: Systima Technologies, Inc.
- Inventors: Richard D. Hreha; Kory K. Evanson; Kristopher K. Aber; Jeffrey R. Josken; Michael D. Rauscher
- Web page: https://patentgrep.com/patent/US12006411B1

## CPC

- C08J 7/123: {Treatment by wave energy or particle radiation (C08J7/18 takes precedence)}
- B29C 71/04: by wave energy or particle radiation {, e.g. for curing or vulcanising preformed articles (during moulding, e.g. in a mould B29C35/08)}
- B64G 1/58: Thermal protection, e.g. heat shields
- C08J 5/243: {using carbon fibres}
- C09K 5/14: Solid materials, e.g. powdery or granular
- F16L 59/028: {Compositions for or methods of fixing a thermally insulating material}
- C08J 2363/00: Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J 2379/00: Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- B64G: COSMONAUTICS; VEHICLES OR EQUIPMENT THEREFOR
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- F16L: PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL

## Abstract

Methods of producing a fiber reinforced polymer matrix composite and a composite thermal protection system formed from the same. The method includes forming a polymerized fiber reinforced composite which including a cured thermoset polymer matrix and at least one reinforcement material. The method further includes treating at least a portion of a first face of the polymerized fiber reinforced composite with electromagnetic radiation to raise the temperature of the portion of the first face to at least 800° C. to produce a surface layer of graphitized carbon and a bulk polymerized fiber reinforced composite representing the untreated polymerized fiber reinforced composite. Further, the surface layer of graphitized carbon has an electrical conductivity of 0.25 S m−1 to 2.5 S m−1 where the electrical conductivity and a thermal conductivity are both greater than those of the bulk polymerized reinforced composite.

## Claims

### Claim 1

A method of producing a fiber reinforced polymer matrix composite, the method comprising:
forming a polymerized fiber reinforced composite, the polymerized fiber reinforced composite comprising a cured thermoset polymer matrix and at least one reinforcement material,
wherein a thermoset polymer forming the cured thermoset polymer matrix comprises at least one polymer represented by chemical formula (I) or (II) or (III)
wherein:
m and n are each an integer greater than or equal to 1,
at least one of R1 or R2 comprises an aromatic moiety, and
X is selected from the group consisting of CH2, NH, O, S, SO2, and combinations thereof, and
wherein the reinforcement material is carbon fiber or ceramic fiber; and
treating at least a portion of a first face of the polymerized fiber reinforced composite with electromagnetic radiation to raise the temperature of the portion of the first face to at least 800° C. to produce a surface layer of graphitized carbon on the first face of the polymerized fiber reinforced composite and a bulk polymerized fiber reinforced composite representing the polymerized fiber reinforced composite not treated with the electromagnetic radiation,
wherein the surface layer of graphitized carbon comprises an electrical conductivity of 0.25 S m−1 to 2.5 S m−1; and
wherein the surface layer of graphitized carbon comprises a thermal conductivity that is greater than a thermal conductivity of the bulk polymerized reinforced composite.

### Claim 2 (depends on 1)

The method of claim 1, wherein the electromagnetic radiation is applied at a power density of 0.05 W/mm2 to 0.75 W/mm2 and delivered at a total energy density to the first face of 0.5 J/mm2 to 2.5 J/mm2.

### Claim 3 (depends on 1)

The method of claim 1, wherein the reinforcement material is carbon fiber.

### Claim 4 (depends on 1)

The method of claim 1, wherein the electromagnetic radiation is produced from a laser with a wavelength range from 690 to 1064 nm.

### Claim 5 (depends on 1)

The method of claim 1, wherein the electromagnetic radiation is generated with a plasma arc lamp operating at a power range from 10,000 W to 25,000 W and a wavelength range from 200 to 1400 nm.

### Claim 6 (depends on 1)

The method of claim 1, wherein the thermal conductivity of the surface layer of graphitized carbon ranges from 25-500 W m−1 K−1.

### Claim 7 (depends on 1)

The method of claim 1, wherein a thickness of the surface layer of graphitized carbon ranges from 0.05 to 2 mm.

### Claim 8 (depends on 1)

The method of claim 1, wherein at least 90% of the first face of the polymerized fiber reinforced composite is treated with the electromagnetic radiation such that the surface layer of graphitized carbon extends across at least 90% of the first face of the polymerized fiber reinforced composite.

### Claim 9 (depends on 1)

The method of claim 1, wherein the first face of the polymerized fiber reinforced composite is treated with the electromagnetic radiation in a defined pattern such that electrically and thermally conductive traces form the surface layer of graphitized carbon.

### Claim 10 (depends on 9)

The method of claim 9, wherein the electrically and thermally conductive traces cover less than 50% of the area of the first face of the polymerized fiber reinforced composite.

### Claim 11 (depends on 1)

The method of claim 1, wherein the reinforcement material is ceramic fiber.

### Claim 12 (depends on 1)

The method of claim 1, wherein the reinforcement material is ceramic fiber selected from the group consisting of silicon carbide fiber, basalt fiber, and their combination.