Infiltrating boron nitride into a carbon-carbon substrate

Patent metadata

Field	Value
Publication number	US-12515997-B2
Application number	US-202318467059-A
Country	US
Kind code	B2
Filing date	Sep 14, 2023
Priority date	Sep 14, 2023
Publication date	Jan 6, 2026
Grant date	Jan 6, 2026

Abstract

A method is provided for forming a carbon/carbon (C/C) disk with boron nitride (BN) doping. Borazine is generated using a set of borazine precursors. Starting carbon fibers are coated or impregnated with the borazine in an inert atmosphere. The starting carbon fibers are needled into layered fabric and the layered fabric is needled into boards from which a preform is cut, the needling and cutting performed in the inert atmosphere. The borazine in the preform is stabilized to convert the borazine to polyborazylene. The polyborazylene in the preform is cured. The polyborazylene in the preform is then crystalized to form BN particulates. The preform with the BN particulates is carbonized and then densified with pyrolytic carbon.

First claim

What is claimed is:

1 . A method for forming a carbon/carbon (C/C) disk with boron nitride (BN) doping, the method comprising:
generating borazine using a set of borazine precursors; coating or impregnating starting carbon fibers with the borazine in an inert atmosphere, wherein an amount of borazine used to coat or infiltrate the starting carbon fibers is between 0.05 percent to 25 percent of a total weight of the starting carbon fibers; needling the starting carbon fibers into layered fabric and then needling the layered fabric into boards from which a preform is cut, the needling and cutting performed in the inert atmosphere; stabilizing the borazine in the preform to convert the borazine to polyborazylene, wherein the stabilizing is performed by heating the preform at a first temperature for a first predetermined time period, wherein the first temperature is between 40° C. (104° F.) to 60° C. (140° F.); curing the polyborazylene in the preform; crystalizing the polyborazylene in the preform to form BN particulates, wherein the crystalizing is performed by heating the preform at a second temperature for a second predetermined time period, causing the polyborazylene to form the BN particulates; and densifying the BN particulates in the preform with pyrolytic carbon.

2 . The method of claim 1 , wherein the coating or impregnating is performed via spraying or dunking in a bath.

3 . The method of claim 1 , wherein the borazine is formed by the method comprising:
mixing the set of borazine precursors with a high-temperature solvent thereby forming a mixture; heating the mixture to a third temperature; capturing off gases emitted by the mixing and heating; and condensing the off gases to liquify the borazine.

4 . The method of claim 3 , wherein the set of borazine precursors comprise ammonium sulfate ((NH 4 ) 2 SO 4 ) and sodium borohydride (NaBH 4 ) and wherein the high-temperature solvent is tetraethylene glycol dimethyl ether, i.e. tetraglyme.

5 . The method of claim 3 , wherein the third temperature is between 135° C. (275° F.) and 150° C. (302° F.).

6 . The method of claim 1 , wherein the first predetermined time period is between 170 hours and 210 hours.

7 . The method of claim 1 , wherein the curing is performed at a third temperature for a third predetermined time period, wherein the third temperature is between 180° C. (356° F.) to 220° C. (428° F.), and wherein the third predetermined time period is between 2 hours and 3 hours.

8 . The method of claim 1 , wherein the second temperature is between 1200° C. (2192° F.) to 2000° C. (3632° F.), and wherein the second predetermined time period is between 2 hours and 5 hours.

9 . A method for forming a carbon/carbon (C/C) disk with boron nitride (BN) doping, the method comprising:
generating borazine using a set of borazine precursors; coating or impregnating a carbonized carbon preform with the borazine in an inert atmosphere, wherein an amount of borazine used to coat or infiltrate the carbonized carbon preform is between 0.05 percent to 25 percent of a total weight of the carbonized carbon preform; stabilizing the borazine in the carbonized carbon preform to convert the borazine to polyborazylene, wherein the stabilizing performed by heating the carbonized carbon preform at a first temperature for a first predetermined time period, wherein the first temperature is between 40° C. (104° F.) to 60° C. (140° F.); curing the polyborazylene in the carbonized carbon preform; crystalizing the polyborazylene in the carbonized carbon preform to form BN particulates, wherein the crystalizing is performed by heating the preform at a second temperature for a second predetermined time period, causing the polyborazylene to form the BN particulates; and densifying the BN particulates in the carbonized carbon preform with pyrolytic carbon.

10 . The method of claim 9 , wherein the coating or impregnating is performed via spraying or dunking in a bath.

11 . The method of claim 9 , wherein the borazine is formed by the method comprising:
mixing the set of borazine precursors with a high-temperature solvent thereby forming a mixture; heating the mixture to a third temperature; capturing off gases emitted by the mixing and heating; and condensing the off gases to liquify the borazine, wherein the set of borazine precursors comprise ammonium sulfate ((NH 4 ) 2 SO 4 ) and sodium borohydride (NaBH 4 ), wherein the high-temperature solvent is tetraethylene glycol dimethyl ether, i.e. tetraglyme, and wherein the third temperature is between 135° C. (275° F.) and 150° C. (302° F.).

12 . The method of claim 9 , wherein the first predetermined time period is between 170 hours and 210 hours.

13 . The method of claim 9 ,
wherein the curing is performed at a third temperature for a third predetermined time period, wherein the third temperature is between 180° C. (356° F.) to 220° C. (428° F.), and wherein the third predetermined time period is between 2 hours and 3 hours, and wherein the second temperature is between 1200° C. (2192° F.) to 2000° C. (3632° F.), and wherein the second predetermined time period is between 2 hours and 5 hours.

14 . The method of claim 9 , wherein the carbonized carbon preform is formed by:
needling uncoated carbon fiber into layered fabric and then needling the layered fabric into boards from which a preform is cut, the needling and cutting performed without BN doping; and carbonizing the preform made of uncoated carbon fibers to form a carbonized carbon preform.

15 . A method for forming a carbon/carbon (C/C) disk with boron nitride (BN) doping, the method comprising:
needling uncoated starting carbon fiber into layered fabric and then needling the layered fabric into boards from which a preform is cut, the needling and cutting performed without BN doping; carbonizing the preform made of uncoated carbon fibers to form a carbonized carbon preform; densifying the carbonized carbon preform with pyrolytic carbon thereby create a densified C/C disk; generating borazine using a set of borazine precursors; coating or impregnating the densified C/C disk with the borazine in an inert atmosphere, wherein an amount of borazine used to coat or infiltrate the densified C/C disk is between 0.05 percent to 25 percent of a total weight of the densified C/C disk; stabilizing the borazine in the densified C/C disk to convert the borazine to polyborazylene, wherein the stabilizing performed by heating the preform at a first temperature for a first predetermined time period, wherein the first temperature is between 40° C. (104° F.) to 60° C. (140° F.); curing the polyborazylene in the densified C/C disk; and crystalizing the polyborazylene in the densified C/C disk to form BN particulates, wherein the crystalizing is performed by heating the preform at a second temperature for a second predetermined time period, causing the polyborazylene to form the BN particulates.

16 . The method of claim 15 , wherein the coating or impregnating is performed via spraying or dunking in a bath.

17 . The method of claim 15 , wherein the borazine is formed by the method comprising:
mixing the set of borazine precursors with a high-temperature solvent thereby forming a mixture; heating the mixture to a third temperature; capturing off gases emitted by the mixing and heating; and condensing the off gases to liquify the borazine, wherein the set of borazine precursors comprise ammonium sulfate ((NH 4 ) 2 SO 4 ) and sodium borohydride (NaBH 4 ), wherein the high-temperature

Assignees

• Goodrich Corp

Inventors

• Jarman Jecee
• Bartolo Lauren

Classifications

• C04B2235/6567

  Treatment time · CPC title

• C04B2235/616

  Liquid infiltration of green bodies or pre-forms · CPC title

• C04B2235/5256

  Two-dimensional, e.g. woven structures · CPC title

• C04B2235/5248

  Carbon, e.g. graphite · CPC title

• C04B2235/486

  Boron containing organic compounds, e.g. borazine, borane or boranyl · CPC title