Alumina ceramic

• US 4,285,732 A
• Filed: 03/11/1980
• Issued: 08/25/1981
• Est. Priority Date: 03/11/1980
• Status: Expired due to Term

• Current Assignee: General Electric Company
• Original Assignee: General Electric Company
• Inventors: Scott, Curtis E., Charles, Richard J., Prochazka, Svante
• Primary Examiner(s): Poer, James
• Application Number:
  US06/129,471
• Time in Patent Office: 532 Days
• Field of Search: 106/57, 106/62, 106/65, 106/73.4
• US Class Current: 501/101
• CPC Class Codes: C04B 2235/3206 Magnesium oxides or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3217 Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
• CPC Class Codes: C04B 2235/3222 Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
• CPC Class Codes: C04B 2235/3244 Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/449 Organic acids, e.g. EDTA, citrate, acetate, oxalate
• CPC Class Codes: C04B 2235/5409 expressed by specific surface values
• CPC Class Codes: C04B 2235/5445 submicron sized, i.e. from 0,1 to 1 micron
• CPC Class Codes: C04B 2235/549 the particle size being expressed by crystallite size or primary particle size
• CPC Class Codes: C04B 2235/608 Green bodies or pre-forms with well-defined density
• CPC Class Codes: C04B 2235/6582 Hydrogen containing atmosphere
• CPC Class Codes: C04B 2235/661 Multi-step sintering
• CPC Class Codes: C04B 2235/77 Density
• CPC Class Codes: C04B 2235/786 Micrometer sized grains, i.e. from 1 to 100 micron
• CPC Class Codes: C04B 2235/80 Phases present in the sintered or melt-cast ceramic products other than the main phase
• CPC Class Codes: C04B 2235/81 Materials characterised by the absence of phases other than the main phase, i.e. single phase materials
• CPC Class Codes: C04B 2235/87 Grain boundary phases intentionally being absent
• CPC Class Codes: C04B 2235/9615 Linear firing shrinkage
• CPC Class Codes: C04B 2235/9623 Ceramic setters properties
• CPC Class Codes: C04B 35/115 Translucent or transparent products
• CPC Class Codes: C04B 35/62655 Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying

Abstract

A particulate dispersion of α-alumina, magnesium oxide and an additive selected from the group consisting of zirconium oxide, hafnium oxide and mixtures thereof, is formed into a green body and sintered in hydrogen producing a theoretically dense ceramic with improved optical transmission properties.

Claims

1. A process for producing an optically translucent polycrystalline alumina sintered body which consists essentially of providing at least a substantially homogeneous dispersion consisting essentially of alumina, MgO or precursor therefor, and an additive selected from the group consisting of ZrO₂, HfO₂, and a mixture thereof or precursors therefor, said alumina ranging in composition from α

-Al₂ O₃ to at least about 80% by weight α

-Al₂ O₃ with the remaining alumina being of polymorphic form other than α

, said MgO being present in an amount ranging from about 0.03% by weight to less than about 0.15% by weight of said alumina, said ZrO₂ being present in an amount ranging from higher than 0.002% by weight up to about 0.07% by weight of said alumina, said HfO₂ being present in an amount ranging from higher than 0.003% by weight up to about 0.12% by weight of said alumina, said mixture of ZrO₂ and HfO₂ being composed of all ratios of ZrO₂ and HfO.sub. 2 and being present in a total amount ranging from higher than 0.002% by weight up to about 0.12% by weight of said alumina, said dispersion having an average crystalline size ranging from about 0.05 micron to less than one micron, forming said dispersion into a green body having a density of at least about 30% of the theoretical density of 3.98 g/cc for alumina, and sintering said body in an atmospheric of hydrogen having a dew point higher than +30°

C. at a sintering temperature ranging from about 1750°

C. to about 1950°

C. producing a sintered body of theoretical density based on the density of 3.98 g/cc for alumina, said precursor decomposing completely below said sintering temperature to form said oxide and by-product gas.

2. The process according to claim 1 wherein said MgO is present in an amount ranging from about 0.03% by weight to about 0.05% by weight of said alumina and said additive is ZrO₂ ranging in amount from about 0.01% by weight to about 0.04% by weight of said alumina.

3. The process according to claim 1 wherein said MgO is present in an amount ranging from about 0.03% by weight to about 0.05% by weight of said alumina and said additive is HfO₂ ranging in amount from about 0.01% by weight to about 0.07% by weight of said alumina.

4. The process according to claim 1 wherein said MgO is present in an amount ranging from about 0.03% by weight to about 0.05% by weight of said alumina and said additive is said mixture of ZrO₂ and HfO₂ ranging in amount from about 0.01% by weight to about 0.07% by weight of said alumina.

5. The process according to claim 1 wherein said sintering temperature ranges from about 1800°

C. to about 1900°

C.

6. The process according to claim 1 wherein said green body is prefired in an oxygen-containing atmosphere at a temperature of from about 800°

C. to about 1300°

C. for at least about one hour.

7. The process according to claim 1 wherein said green body is heated at a temperature ranging from about 800°

C. to about 1300°

C. in a wet hydrogen atmosphere having a dew point of at least about 0°

C. to eliminate impurities therein which would have a significantly deleterious effect on the optical translucency of said sintered body.

8. An optically translucent polycrystalline alumina sintered body of theoretical density based on the density of 3.98 g/cc for alumina consisting essentially of alumina, magnesium and a component selected from the group consisting of zirconium, hafnium and a mixture thereof, said magnesium being present in an amount equivalent to from about 0.03% MgO by weight to less than about 0.15% MgO by weight of said sintered body, said zirconium being present in an amount equivalent to from higher than about 0.002% ZrO₂ by weight up to about 0.07% ZrO₂ by weight of said sintered body, said hafnium being present in an amount equivalent to from higher than about 0.003% HfO₂ by weight up to about 0.12% HfO₂ by weight of said sintered body, said mixture thereof being composed of all ratios of said zirconium and hafnium and being present in an amount equivalent to from higher than 0.002% of the di-oxides thereof by weight up to about 0.12% of the di-oxides thereof by weight of said sintered body, said sintered body ranging from a single phase to one composed of a primary phase and secondary phase ranging up to but less than 1% by volume of the total volume of said sintered body, said sintered body having an average grain size ranging from about 15 microns to about 100 microns.

9. The optically translucent polycrystalline alumina sintered body according to claim 8 wherein said component is zirconium.

10. The optically translucent polycrystalline alumina sintered body according to claim 8 wherein said component is hafnium.

11. The optically translucent polycrystalline alumina sintered body according to claim 8 wherein said component is said mixture of zirconium and hafnium.

12. An optically translucent polycrystalline alumina sintered body of theoretical density based on the density of 3.98 g/cc for alumina consisting essentially of α

-Al₂ O₃, magnesium and zirconium, said magnesium being equivalent to about 0.03% MgO by weight to about 0.05% MgO by weight of said sintered body, said zirconium being equivalent to from about 0.01% ZrO₂ by weight to about 0.04% ZrO₂ by weight of said sintered body, said sintered body ranging from a single phase to one composed of a primary phase and secondary phase ranging up to but less than 1% by volume of the total volume of said sintered body, said sintered body having an average grain size ranging from about 20 microns to about 50 microns.

13. An optically translucent polycrystalline alumina sintered body of theoretical density based on the density of 3.98 g/cc for alumina consisting essentially of α

-Al₂ O₃, magnesium and hafnium, said magnesium being equivalent to about 0.03% MgO by weight to about 0.05% MgO by weight of said sintered body, said hafnium being equivalent to from about 0.01% HfO₂ by weight to about 0.07% HfO₂ by weight of said sintered body, said sintered body ranging from a single phase to one composed of a primary phase and secondary phase ranging up to but less than 1% by volume of the total volume of said sintered body, said sintered body having an average grain size ranging from about 20 microns to about 50 microns.

14. An optically translucent polycrystalline sintered alumina body of theoretical density based on the density of 3.98 g/cc for alumina consisting essentially of α

-Al₂ O₃, magnesium, zirconium and hafnium, said magnesium being equivalent to about 0.03% by weight to about 0.05% MgO by weight of said sintered body, the total amount of said zirconium and hafnium being equivalent to from about 0.01% of the di-oxides thereof by weight to about 0.07% of the di-oxides thereof by weight of said sintered body, said sintered body ranging from a single phase to one composed of a primary phase and secondary phase ranging up to but less than 1% by volume of the total volume of said sintered body, said sintered body having an average grain size ranging from about 20 microns to about 50 microns.