Claims
- 1. A method of manufacturing an aluminum nitride, which comprises the steps of:
- (a) preparing a mixed gas consisting essentially of an ammonia gas and at least 0.5% by volume of a hydrocarbon gas;
- (b) calcining .gamma.-Al.sub.2 O.sub.3 or a precursor thereof at a temperature of 300.degree. to 1,100.degree. C. so as to prepare the .gamma.-Al.sub.2 O.sub.3 having a moisture content of 1 weight % or less;
- (c) heating the calcined .gamma.-Al.sub.2 O.sub.3 in said mixed gas at a temperature of 1,200.degree. to 1,700.degree. C., thereby preparing porous aluminum nitride having a specific surface area of 10 m.sup.2 /g or more; and
- (d) heat-treating the porous aluminum nitride in an atmosphere of an ammonia gas or a mixed gas of an ammonia gas and an inert gas at 1600.degree. to 2000.degree. C., so as to make contents of both carbon and oxygen contained in the aluminum nitride 1 weight % or less.
- 2. A method of manufacturing an aluminum nitride, which comprises the steps of:
- (a) preparing a mixed gas consisting essentially of an ammonia gas and at least 0.5% by volume of a hydrocarbon gas;
- (b) calcining .gamma.-Al.sub.2 O.sub.3 or a precursor thereof at a temperature of 300.degree. to 1,100.degree. C. so as to prepare the .gamma.-Al.sub.2 O.sub.3 having a moisture content of 1 weight % or less;
- (c) heating the calcined .gamma.-Al.sub.2 O.sub.3 in said mixed gas at a temperature of 1,200.degree. to 1,700.degree. C., thereby preparing porous aluminum nitride having a specific surface area of 10 m.sup.2 /g or more;
- (d) subjecting the porous aluminum nitride to an oxidation-decarbonization in an atmosphere at 600.degree. to 800.degree. C.; and
- (e) heat-treating the porous aluminum nitride in an atmosphere of an inert gas at 1,600.degree. to 2000.degree. C., so as to make contents of both carbon and oxygen contained in the aluminum nitride 1 weight % or less.
- 3. The method according to claim 1, wherein said hydrocarbon is at least one compound selected from the group consisting of propane, methane, ethane and butane.
- 4. The method according to claim 1, wherein the heating temperature for preparing the porous aluminum nitride is in the range of 1,300.degree. to 1460.degree. C.
- 5. The method according to claim 1, wherein the .gamma.-Al.sub.2 O.sub.3 is in the form of particle or flake.
- 6. The method according to claim 1, wherein the precursor of .gamma.-Al.sub.2 O.sub.3 is selected from the group consisting of aluminum alkoxide, aluminum sulfate, aluminum alum, ammonium aluminum carbonate, aluminum hydroxy chloride and boehmite.
- 7. The method according to claim 1, wherein the .gamma.-Al.sub.2 O.sub.3 is formed using, as a sole alumina source or as part of alumina source, aluminum hydroxy chloride.
- 8. The method according to claim 1, wherein a temperature for heat-treating the porous aluminum nitride in the atmosphere of the ammonia gas, or the mixed gas of the ammonia gas and the inert gas, is 1,600.degree. to 1800.degree. C.
- 9. The method according to claim 2, wherein a temperature for heat-treating the porous aluminum nitride in the atmosphere of the inert gas, is 1,600.degree. to 1800.degree. C.
- 10. A method of manufacturing aluminum nitride fibers, which comprises the steps of:
- (a) preparing a mixed gas consisting essentially of an ammonia gas and at least 0.5% by volume of a hydrocarbon gas;
- (b) dispersing a precursor of .gamma.-Al.sub.2 O.sub.3 in a dispersion containing a binder and one material selected from the group consisting of colloidal silica, colloidal alumina and colloidal zirconia;
- (c) concentrating said dispersion containing said precursor dispersed therein;
- (d) spinning short fibers from the concentrated dispersion placed in a centrifugal spinning machine by rotating the centrifugal spinning machine;
- (e) drying the spun short fibers;
- (f) calcining the dried short fibers at a temperature of 300.degree. to 1,100.degree. C. so as to make a moisture content 1 weight % or less;
- (g) heat-treating the calcined short fibers in said mixed gas consisting essentially of a hydro-carbon gas and an ammonia gas at a temperature of 1,200.degree. to 1,700.degree. C., so as to form porous aluminum nitride fibers having a specific surface area of 10 m.sup.2 /g or more; and
- (h) heat-treating the porous aluminum nitride fibers in an atmosphere of an ammonia gas, or a mixed gas of an ammonia gas and an inert gas, at 1,600.degree. to 2000.degree. C., so as to make contents of both carbon and oxygen contained in the aluminum nitride fibers 1 weight % or less.
- 11. A method of manufacturing aluminum nitride fibers, which comprises the steps of:
- (a) preparing a mixed gas consisting essentially of an ammonia gas and at least 0.5% by volume of a hydrocarbon gas;
- (b) dispersing a precursor of .gamma.-Al.sub.2 O.sub.3 in a dispersion containing a binder and one material selected from the group consisting of colloidal silica, colloidal alumina and colloidal zirconia;
- (c) concentrating said dispersion containing said precursor dispersed therein;
- (d) spinning short fibers from the concentrated dispersion placed in a centrifugal spinning machine by rotating the centrifugal spinning machine;
- (e) drying the spun short fibers;
- (f) calcining the dried short fibers at a temperature of 300.degree. to 1,100.degree. C. so as to make a moisture content 1 weight % or less;
- (g) heat-treating the calcined short fibers in said mixed gas consisting essentially of a hydrocarbon gas and an ammonia gas at a temperature of 1,200.degree. to 1,700.degree. C., so as to form porous aluminum nitride fibers having a specific surface area of 10 m.sup.2 /g or more;
- (h) subjecting the porous aluminum nitride fibers to an oxidation-carbonization in an atmophere at a temperature of 600.degree. to 800.degree. C.; and
- (g) heat-treating the porous aluminum nitride fibers in an atmosphere of an inert gas, at 1,600.degree. to 2000.degree. C., so as to make contents of both carbon and oxygen contained in the aluminum nitride fibers 1 weight % or less.
- 12. The method according to claim 10, wherein said hydrocarbon gas is at least one compound selected from the group consisting of propane, methane, ethane and butane.
- 13. The method according to claim 10, wherein said temperature for preparing the porous aluminum nitride fibers is in the range of 1,300.degree. to 1,460.degree. C.
- 14. The method of manufacturing aluminum nitride fibers according to claim 10, wherein the precursor of .gamma.-Al.sub.2 O.sub.3 is formed using, as a sole alumina source or as part of alumina source, aluminum hydroxy chloride.
- 15. The method according to claim 2, wherein said hydrocarbon is at least one compound selected from the group consisting of propane, methane, ethane and butane.
- 16. The method according to claim 2, wherein the heating temperature for preparing the porous aluminum nitride is in the range of 1,300.degree. to 1,460.degree. C.
- 17. The method according to claim 2, wherein the precursor of .gamma.Al.sub.2 O.sub.3 is selected from the group consisting of aluminum alkoxide, aluminum sulfate, aluminum alum, ammonium aluminum carbonate, aluminum hydroxy chloride and boehmite.
- 18. The method according to claim 2, wherein the .gamma.-Al.sub.2 O.sub.3 is formed using, as a sole alumina source or as part of alumina source, aluminum hydroxy chloride.
- 19. The method according to claim 11, wherein said hydrocarbon gas is at least one compound selected from the group consisting of propane, methane, ethane and butane.
- 20. The method according to claim 11, wherein said temperature for preparing the porous aluminum nitride fibers is in the range of 1,300.degree. to 1,460.degree. C.
- 21. The method of manufacturing aluminum nitride fibers according to claim 11, wherein the precursor of .gamma.-Al.sub.2 O.sub.3 is formed using, as a sole alumina source or as part of alumina source, aluminum hydroxy chloride.
Priority Claims (1)
Number |
Date |
Country |
Kind |
7-206027 |
Aug 1995 |
JPX |
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of U.S. patent application Ser. No. 8/689,170 filed Aug. 6, 1996, now abandoned.
US Referenced Citations (5)
Foreign Referenced Citations (2)
Number |
Date |
Country |
2-300319 |
Dec 1990 |
JPX |
6-330412 |
Nov 1994 |
JPX |
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
689170 |
Aug 1996 |
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