Heat-resistant composite material production method and production device

Patent metadata

Field	Value
Publication number	US-10221104-B2
Application number	US-201615165676-A
Country	US
Kind code	B2
Filing date	May 26, 2016
Priority date	Feb 25, 2014
Publication date	Mar 5, 2019
Grant date	Mar 5, 2019

Abstract

A mixed gas containing a precursor gas, an additive gas and a carrier gas is supplied to a preform stored in an electric furnace, and silicon carbide is deposited by chemical vapor deposition or chemical vapor phase impregnation to form a film. The preform includes multiple fiber bundles, and the fiber bundles include multiple fibers. This heat-resistant composite material includes a ceramic fiber preform impregnated with silicon carbide, and producing the composite material involves a step in which silicon carbide is deposited between the fibers to integrate the fibers which configure the fiber bundles, and a step in which silicon carbide is deposited between the fiber bundles to integrate the fiber bundles. Hereby, uniformity of embedding and growth rate of the silicon carbide film are both attained.

First claim

What is claimed is:

1. A method of manufacturing a heat-resistant composite material, the method comprising:
treating a preform comprising a plurality of fiber bundles, each fiber bundle having a plurality of fibers, by:
wrapping a woven fabric having a predetermined thickness around an outer circumference of the preform to provide a wrapped preform;
depositing silicon carbide between the fibers of the wrapped preform to integrate the fibers constituting each fiber bundle to provide a fiber-integrated wrapped preform;
removing the woven fabric from the fiber-integrated wrapped preform to provide a fiber-integrated preform; and
depositing silicon carbide between the fiber bundles of the fiber-integrated preform to integrate the fiber bundles,
wherein said depositing silicon carbide between the fibers of the wrapped preform is accomplished by allowing precursor gas, additive gas, and carrier gas to flow in a reaction furnace accommodating the wrapped preform,
wherein said depositing silicon carbide between the fiber bundles of the fiber-integrated preform is accomplished by allowing precursor gas, additive gas, and carrier gas to flow in a reaction furnace accommodating the fiber-integrated preform.

2. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
in said depositing silicon carbide between the fibers of the wrapped preform to integrate the fibers constituting each fiber bundle, the ratio C/C 0 of concentration C of the precursor gas at the center of the fiber bundles to initial concentration C 0 of the precursor gas supplied to the reaction furnace is in a range from 0.2 to 0.3.

3. The method of manufacturing a heat-resistant composite material according to claim 2 , wherein
the ratio C/C 0 is in a range from 0.24 to 0.26.

4. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
in said depositing silicon carbide between the fibers of the wrapped preform to integrate the fibers constituting each fiber bundle, a growth temperature of the reaction furnace is in a range from 800 to 1000° C., and a total pressure of the precursor gas, additive gas, and carrier gas in the reaction furnace is in a range of 4 to 6 Torr.

5. The method of manufacturing a heat-resistant composite material according to claim 4 , wherein
the growth temperature is in a range from 850 to 950° C., and the total pressure is in a range of 4.5 to 5.5 Torr.

6. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
in said depositing silicon carbide between the fiber bundles of the fiber-integrated preform to integrate the fiber bundles, the ratio C/C 0 of concentration C of the precursor gas at the center of the fiber-integrated preform to the initial concentration C 0 of the precursor gas supplied to the reaction furnace is in a range from 0.2 to 0.3.

7. The method of manufacturing a heat-resistant composite material according to claim 6 , wherein
the ratio C/C 0 is in a range from 0.24 to 0.26.

8. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
in said depositing silicon carbide between the fiber bundles of the fiber-integrated preform to integrate the fiber bundles, a growth temperature of the reaction furnace is in a range from 800 to 1000° C., and a total pressure of the precursor gas, additive gas, and carrier gas in the reaction furnace is in a range of 5 to 110 Torr.

9. The method of manufacturing a heat-resistant composite material according to claim 8 , wherein
the growth temperature is in a range from 850 to 950° C., and the total pressure is in a range of 5 to 105 Torr.

10. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the woven fabric is wound around the outer circumference of the preform to provide the wrapped preform.

11. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the preform is made of woven fabric, and the woven fabric is made of the same material as that of the preform.

12. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the precursor gas used to deposit silicon carbide between the fibers of the wrapped preform and the precursor gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform each comprise at least one of methyltrichlorosilane, dimethyldichlorosilane, tetramethylsilane, and trimethylchlorosilane.

13. The method of manufacturing a heat-resistant composite material according to claim 12 , wherein
the precursor gas used to deposit silicon carbide between the fibers of the wrapped preform comprises methyltrichlorosilane, and
the precursor gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform comprises at least one of dimethyldichlorosilane, tetramethylsilane, and trimethylchlorosilane.

14. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
the carrier gas used to deposit silicon carbide between the fibers of the wrapped preform, and the carrier gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform, each comprise at least one of hydrogen, nitrogen, helium, and argon.

15. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
the additive gas used to deposit silicon carbide between the fibers of the wrapped preform, and the additive gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform, each comprise at least one of hydrogen chloride, monochloromonomethylsilane, methyldichlorosilane, methyltrichlorosilane, dimethylmonochlorosilane, dimethyldichlorosilane, trimethylmonochlorosilane, monochlorosilane, dichlorosilane, trichlorosilane, tetrachlorosilane, chlorodisilane, dichlorodisilane, hexachlorodisilane, octachlorotrisilane, monochloromethane, dichloromethane, chloroform, tetrachloromethane, monochloroacetylene, dichloroacetylene, monochloroethylene, dichloroethylene, trichloroethylene, tetrachloroethylene, monochloroethane, dichloroethane, trichloroethane, tetrachloroethane, pentachloroethane, hexachloroethane, monochloropropane, dichloropropane, trichloropropane, tetrachloropropane, pentachloropropane, hexachloropropane, heptachloropropane, octachloropropane, and chlorine molecules.

16. The method of manufacturing a heat-resistant composite material according to claim 15 , wherein the additive gas used to deposit silicon carbide between the fibers of the wrapped preform, and the additive gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform, comprises hydrogen chloride.

17. The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the precursor gas used to deposit silicon carbide between the fibers of the wrapped preform, and the precursor gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform, comprises methyltrichlorosilane, and the carrier gas used to deposit silicon carbide between the fibers of the wrapped preform, and the carrier gas used to deposit silicon carbide between the fiber bundles of the fiber-integrated preform, comprises hydrogen.

18. The method of manufacturing a heat-resistant composite material according to claim 17 , wherein a molar ratio of hydrogen to methyltrichlorosilane is in a range from 1.5 to 2.5.

19. The method of manufacturin

Assignees

• Ihi Corp
• Univ Tokyo

Inventors

• Nakamura Takeshi
• Ishizaki Masato
• Hotozuka Kozue
• Fukushima Yasuyuki
• Shimogaki Yukihiro
• Momose Takeshi
• Sugiura Hidetoshi
• Shima Kohei
• Funato Yuichi

Classifications

• C04B35/565

  based on silicon carbide · CPC title

• C04B2235/5248

  Carbon, e.g. graphite · CPC title

• C23C16/325

  Silicon carbide · CPC title

• C04B41/4531 Primary

  by C.V.D. · CPC title

• C04B2235/5252

  having a specific pre-form · CPC title