Heat-resistant composite material production method and production device
US-2016305015-A1 · Oct 20, 2016 · US
US11229893B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11229893-B2 |
| Application number | US-201916239845-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jan 4, 2019 |
| Priority date | Jul 6, 2016 |
| Publication date | Jan 25, 2022 |
| Grant date | Jan 25, 2022 |
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Provided is a method of producing a silicon compound material, including the steps of: storing a silicon carbide preform in a reaction furnace; supplying a raw material gas containing methyltrichlorosilane to the reaction furnace to infiltrate the preform with silicon carbide; and controlling and reducing a temperature of a gas discharged from the reaction furnace at a predetermined rate to subject the gas to continuous thermal history, to thereby decrease generation of a liquid or solid by-product derived from the gas.
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What is claimed is: 1. A method of producing a silicon compound material, comprising: storing a silicon carbide preform in a reaction furnace; supplying a raw material gas containing methyltrichlorosilane to the reaction furnace to infiltrate the preform with silicon carbide; and reducing a temperature of a gas discharged from the reaction furnace to a predetermined temperature within a range of 500° C. or more and less than 950° C. at a predetermined rate, and subsequently retaining the temperature of the gas at the predetermined temperature, thereby decreasing generation of a liquid or solid by-product derived from the gas. 2. A method of producing a silicon compound material according to claim 1 , wherein the predetermined temperature is within a range of 600° C. or more and less than 800° C. 3. A method of producing a silicon compound material according to claim 2 , wherein the gas discharged from the reaction furnace is retained at the predetermined temperature for a predetermined time period within a range of from 0 seconds to 8 seconds. 4. A method of producing a silicon compound material according to claim 2 , wherein the temperature of the gas discharged from the reaction furnace is reduced to the predetermined temperature such that the temperature of the gas is changed to a plurality of temperatures in a stepwise manner. 5. A method of producing a silicon compound material according to claim 2 , wherein the liquid or solid by-product comprises a higher-chlorosilane. 6. A method of producing a silicon compound material according to claim 2 , wherein the reducing of the temperature of the gas discharged from the reaction furnace and the retaining of the temperature of the gas are performed such that SiCl 2 serving as a precursor of the liquid or solid by-product is converted into a stable substance. 7. A method of producing a silicon compound material according to claim 1 , wherein the gas discharged from the reaction furnace is retained at the predetermined temperature for a predetermined time period within a range of from 0 seconds to 8 seconds. 8. A method of producing a silicon compound material according to claim 1 , wherein the temperature of the gas discharged from the reaction furnace is reduced to the predetermined temperature such that the temperature of the gas is changed to a plurality of temperatures in a stepwise manner. 9. A method of producing a silicon compound material according to claim 1 , wherein the liquid or solid by-product comprises a higher-chlorosilane. 10. A method of producing a silicon compound material according to claim 1 , wherein the reducing of the temperature of the gas discharged from the reaction furnace and the retaining of the temperature of the gas are performed such that SiCl 2 serving as a precursor of the liquid or solid by-product is converted into a stable substance. 11. A method of producing a silicon compound material according to claim 10 , wherein the stable substance comprises at least one selected from the group consisting of methyltrichlorosilane, dimethyldichlorosilane, disilane, dichlorosilane, trichlorosilane, and tetrachlorosilane. 12. A method of producing a silicon compound material according to claim 1 , wherein the gas discharged from the reaction furnace contains hydrogen. 13. A method of producing a silicon compound material according to claim 1 , wherein the temperature of the gas discharged from the reaction furnace is retained at the predetermined temperature immediately after the temperature is reduced to the predetermined temperature, wherein the predetermined temperature is within a range of 600° C. or more and less than 800° C., and wherein the gas discharged from the reaction furnace is retained at the predetermined temperature for a predetermined time period which is greater than 0 second and 8 seconds or less. 14. A method of producing a silicon compound material, comprising: storing a silicon carbide preform in a reaction furnace; supplying a raw material gas containing methyltrichlorosilane to the reaction furnace to infiltrate the preform with silicon carbide; and reducing a temperature of a gas discharged from the reaction furnace to a predetermined temperature at a predetermined rate while adding an additive gas to the gas discharged from the reaction furnace, and subsequently retaining the temperature of the gas to which the additive gas has been added at the predetermined temperature, thereby decreasing generation of a liquid or solid by-product derived from the gas discharged from the reaction furnace. 15. A method of producing a silicon compound material according to claim 14 , wherein the additive gas is added such that an amount of substance of the additive gas is larger than an amount of substance of the liquid or solid by-product. 16. A method of producing a silicon compound material according to claim 14 , wherein the additive gas is added such that an amount of substance of chlorine is larger than an amount of substance of silicon contained in the liquid or solid by-product. 17. A method of producing a silicon compound material according to claim 14 , wherein the temperature of the gas discharged from the reaction furnace is retained at the predetermined temperature using a reforming furnace, such that a time period for which the gas discharged from the reaction furnace is retained at the predetermined temperature is a residence time of the gas in the reforming furnace. 18. A method of producing a silicon compound material according to claim 14 , wherein the predetermined temperature is within a range of 200° C. or more and less than 1,100° C. 19. A method of producing a silicon compound material according to claim 14 , wherein the predetermined temperature is within a range of 750° C. or more and less than 850° C. 20. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises a molecule containing chlorine. 21. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises at least one selected from the group consisting of a nitrogen gas, a hydrogen gas, hydrogen chloride, chloromethane, tetrachloromethane, trichloroethylene, trichloroethane, ethylene, ethanol, acetone, methanol, water vapor, dichloromethane, and chloroform. 22. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises chloromethane or dichloromethane, and wherein the gas discharged from the reaction furnace to which the additive gas has been added is retained at the predetermined temperature for a time period of 0.08 second or more. 23. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises chloromethane or dichloromethane, and wherein the gas discharged from the reaction furnace to which the additive gas has been added is retained at the predetermined temperature for a time period of 1 second or more. 24. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises chloromethane, and wherein the additive gas is added such that an amount of substance of chloromethane to be added is 1.0 time or more as large as an amount of substance of methyltrichlorosilane in the raw material gas. 25. A method of producing a silicon compound material according to claim 14 , wherein the additive gas comprises chl
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