# US 11,440,851 B1 · Method of making carbon matrix composite from high temperature polymer matrix fiber-reinforced composites

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- Number: US 11,440,851 B1
- Document ID: US11440851B1
- Status: Granted
- Kind: B1
- Application number: 16/275,630
- Filed: 2019-02-14
- Granted: 2022-09-13
- Earliest claimed: 2018-02-14
- Assignees: Systima Technologies, Inc.
- Applicants: Jalapeno Holdings, LLC
- Inventors: Richard D. Hreha; Kristopher K. Aber; Joel P. Brubaker; Kristin M. Cable; Michael D. Rauscher
- Web page: https://patentgrep.com/patent/US11440851B1

## CPC

- B32B 18/00: Layered products essentially comprising ceramics, e.g. refractory products
- C04B 35/83: Carbon fibres in a carbon matrix
- C04B 35/522: {Graphite (C04B35/536 takes precedence)}
- C04B 35/64: Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F})
- C08J 5/042: {with carbon fibres}
- C04B 2235/422: Carbon
- C04B 2235/5248: Carbon, e.g. graphite
- C04B 2235/5252: having a specific pre-form
- C04B 2235/616: Liquid infiltration of green bodies or pre-forms
- C04B 2235/6562: Heating rate
- C04B 2235/6565: Cooling rate
- C04B 2235/6567: Treatment time
- C04B 2235/658: Atmosphere during thermal treatment
- C04B 2235/661: Multi-step sintering
- C04B 2235/80: Phases present in the sintered or melt-cast ceramic products other than the main phase
- C04B 2235/96: Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B 2237/385: Carbon or carbon composite
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- 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)

## 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 R1 or R2 comprises an aromatic moiety, and X is selected from the group consisting of CH2, NH, O, S, SO2, 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

### Claim 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 R1 or R2 comprises an aromatic moiety, and
X is selected from the group consisting of CH2, NH, O, S, SO2, 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.

### Claim 2 (depends on 1)

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

### Claim 3 (depends on 1)

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.

### Claim 4 (depends on 1)

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.

### Claim 5 (depends on 1)

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

### Claim 6 (depends on 1)

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

### Claim 7 (depends on 1)

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.

### Claim 8 (depends on 1)

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.

### Claim 9 (depends on 4)

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.

### Claim 10 (depends on 1)

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

### Claim 11 (depends on 1)

The method of claim 1, wherein R1, R2, or both comprise one or more of a phenyl group, a naphthyl group, a benzyl group, or a 4-cyanophenyl group.

### Claim 12 (depends on 1)

The method of claim 1, wherein R1, R2, 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.

### Claim 13 (depends on 1)

The method of claim 1, wherein R1, R2, 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.

### Claim 14 (depends on 1)

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.

### Claim 15 (depends on 1)

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.

### Claim 16 (depends on 15)

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.

### Claim 17 (depends on 1)

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.

### Claim 18 (depends on 1)

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.

### Claim 19 (depends on 4)

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.

### Claim 20 (depends on 1)

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