Heat-resistant composite material production method and production device

Patent metadata

Field	Value
Publication number	US-2016297716-A1
Application number	US-201615165676-A
Country	US
Kind code	A1
Filing date	May 26, 2016
Priority date	Feb 25, 2014
Publication date	Oct 13, 2016
Grant date	—

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 producing a heat-resistant composite material which uses chemical vapor deposition or chemical vapor infiltration to allow precursor gas, additive gas, and carrier gas to flow in a reaction furnace accommodating a preform and deposit silicon carbide on the preform for film formation, the preform including a plurality of fiber bundles, each having a plurality of fibers, the method comprising the steps of:
depositing silicon carbide between the fibers to integrate the fibers constituting each fiber bundle; and depositing silicon carbide between the fiber bundles to integrate the fiber bundles.

2 . The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
in the step of integrating the fibers, the ratio C/C 0 of concentration C of the precursor gas at the center of the fibers 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 the step of integrating the fibers, growth temperature is in a range from 800 to 1000° C., and total pressure of the precursor gas, additive gas, and carrier gas 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 the step of integrating the fiber bundles, the ratio C/C 0 of concentration C of the precursor gas at the center of the fiber bundles 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 the step of integrating the fiber bundles, growth temperature is in a range from 800 to 1000° C., and total pressure of the precursor gas, additive gas, and carrier gas 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 , further comprising:
a step of providing woven fabric having a predetermined thickness to wrap around the outer circumference of the preform before the step of integrating the fibers; and a step of removing the woven fabric from the preform after the step of integrating the fibers constituting the fiber bundles and before the step of integrating the fiber bundles.

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

12 . The method of manufacturing a heat-resistant composite material according to claim 10 , wherein the preform is made of woven fabric, and the woven fabric provided on the circumference of the preform is made of the same material as that of the preform.

13 . The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the precursor gas contains at least any one of methyltrichlorosilane, dimethyldichlorosilane, tetramethylsilane, and trimethylchlorosilane.

14 . The method of manufacturing a heat-resistant composite material according to claim 13 , wherein
the precursor gas contains methyltrichlorosilane in the step of integrating the fibers, and the precursor gas contains at least any one of dimethyldichlorosilane, tetramethylsilane, and trimethylchlorosilane in the step of integrating the fiber bundles.

15 . The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
the carrier gas contains at least one of hydrogen, nitrogen, helium, and argon.

16 . The method of manufacturing a heat-resistant composite material according to claim 1 , wherein
the additive gas contains 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.

17 . The method of manufacturing a heat-resistant composite material according to claim 16 , wherein the additive gas contains hydrogen chloride.

18 . The method of manufacturing a heat-resistant composite material according to claim 1 , wherein the precursor gas contains methyltrichlorosilane, and the carrier gas contains hydrogen.

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

20 . The method of manufacturing a heat-resistant composite material according to claim 19 , wherein the molar ratio of hydrogen to methyltrichlorosilane is in a range from 1.9 to 2.1.

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

• C04B41/87

  Ceramics · CPC title

• C04B41/009

  characterised by the material treated · CPC title

• C04B2235/614

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

• C23C16/325

  Silicon carbide · CPC title

• C04B41/5059

  Silicon carbide · CPC title