Alpha Al2O3 and Ti2O3 protective coatings on aluminide substrates
First Claim
1. A process for forming a specific reactive element barrier on an aluminum containing substrate, the process comprising:
- creating a dry air atmosphere, which includes nitrogen and oxygen gas, with a concentration of water vapor below about 750 ppm at a temperature above about 550°
C. contiguous to a surface of the substrate on which the barrier layer is to be formed;
maintaining the temperature above 550°
C. and water vapor concentration below about 750 ppm;
reacting the water vapor in the dry air atmosphere with specific reactive elements at the substrate surface to form a specific reactive element oxide barrier layer which is strongly bonded to the substrate surface, said barrier layer including an aluminum oxide layer at the substrate/barrier layer interface.
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Abstract
In accordance with one aspect of the present invention, a process for forming a specific reactive element barrier on a titanium and aluminum containing substrate is provided. The process includes creating a dry air atmosphere with a concentration of water vapor below about 750 ppm at a temperature above about 550° C. contiguous to a surface of the substrate on which the barrier layer is to be formed. The temperature is maintained above 550° C. and the water vapor concentration is maintained below about 100 ppm while the water vapor in the dry air atmosphere is reacted with specific reactive elements at the substrate surface. The reaction forms a specific reactive element oxide barrier layer which is strongly bonded to the substrate surface. The barrier layer includes an aluminum oxide layer at the substrate/barrier layer interface and a second oxide layer at a barrier layer/atmosphere interface.
33 Citations
36 Claims
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1. A process for forming a specific reactive element barrier on an aluminum containing substrate, the process comprising:
-
creating a dry air atmosphere, which includes nitrogen and oxygen gas, with a concentration of water vapor below about 750 ppm at a temperature above about 550°
C. contiguous to a surface of the substrate on which the barrier layer is to be formed;
maintaining the temperature above 550°
C. and water vapor concentration below about 750 ppm;
reacting the water vapor in the dry air atmosphere with specific reactive elements at the substrate surface to form a specific reactive element oxide barrier layer which is strongly bonded to the substrate surface, said barrier layer including an aluminum oxide layer at the substrate/barrier layer interface. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8)
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9. A process for forming a specific reactive element barrier on an aluminum and titanium containing substrate, the process comprising:
-
creating a dry air atmosphere with a concentration of water vapor below about 750 ppm at a temperature above about 550°
C. contiguous to a surface of the substrate on which the barrier layer is to be formed;
reacting the water vapor in the dry air atmosphere with specific reactive elements at the substrate surface to form a specific reactive element oxide barrier layer which is strongly bonded to the substrate surface, said barrier layer including an aluminum oxide layer including crystalline α
-Al2O3 and a titanium oxide layer including crystalline Ti2O3, the crystalline α
-Al2O3 and the Ti2O3 having like lattice constants. - View Dependent Claims (10, 11)
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12. A process for forming a specific reactive element barrier on an aluminum and titanium containing substrate, the process comprising:
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exposing the substrate to atmospheric air with a concentration of water vapor below about 750 ppm at a temperature greater than about 500°
C. contiguous to a surface of the substrate on which the barrier layer is to be formed;
dissociating oxygen in said water vapor;
reacting the dissociated oxygen with aluminum and titanium in the substrate to form aluminum and titanium oxide layers, the reacting step including forming crystalline fibers of TiO2 titanium oxide. - View Dependent Claims (13, 14, 15, 16, 17, 18, 19)
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20. A process for forming a specific reactive element barrier on an aluminum containing substrate, the processing comprising:
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creating a dry air atmosphere with a concentration of water vapor below about 100 ppm at a temperature above about 550°
C. contiguous to a surface of the substrate on which the barrier layer is to be formed;
reacting oxygen dissociated from the water vapor in the dry air atmosphere with specific reactive elements at the substrate surface to form a specific reactive element oxide barrier layer which is strongly bonded to the substrate surface, said barrier layer including an aluminum oxide layer at a substrate/barrier layer interface and a second oxide layer at a barrier layer/atmosphere interface; and
reacting sulfur at the substrate surface with hydrogen produced by dissociation of water vapor to form hydrogen sulfide gas; and
removing the hydrogen sulfide gas from the substrate surface.
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21. A product with a specific reactive element barrier on substrate, the product comprising:
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a substrate containing aluminum and titanium;
an α
-Al2O3 aluminum oxide layer bonded to the aluminum containing substrate; and
a Ti2O3 titanium oxide layer bonded to the Al2O3 layer. - View Dependent Claims (22, 23, 24)
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25. A process for forming a specific reactive element by layer on a titanium aluminide substrate, the process comprising:
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creating a gaseous/water vapor atmosphere with a concentration of water vapor below about 750 ppm at a temperature above about 550°
C. contiguous to a surface of the titanium aluminide substrate on which the barrier layer is to be formed;
while maintaining the temperature above about 550°
C. and water vapor concentration below about 750 ppm, reacting the oxygen of the water vapor with specific reactive elements at the titanium aluminide substrate surface until;
α
-Al2O3 is formed directly on the substrate surface in preference to titanium oxide to form a crystalline α
-Al2O3 layer at a substrate/barrier layer interface;
titanium atoms from titanium oxide are reduced with aluminum and the titanium atoms diffuse outward through the α
-Al2O3 layer;
oxidizing the titanium atoms that have diffused through the α
-Al2O3 layer to form a crystalline Ti2O3 layer at a barrier layer/gas interface, the crystalline α
-Al2O3 and Ti2O3 have like lattice structures; and
exposing the substrate and the α
-Al2O3 and Ti2O3 layers to atmospheric air with a water vapor content above 750 ppm at a temperature greater than about 500°
C. to reach remaining titanium atoms to form TiO2 fibers. - View Dependent Claims (26, 27)
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28. A barrier layer protected titanium aluminide material substrate comprising:
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a crystalline α
-Al2O3 layer bonded to a surface of the titanium aluminide substrate;
a crystalline Ti2O3 layer bonded to the α
-Al2O3 layer; and
crystalline TiO2 fibers in the α
-Al2O3 and Ti2O3 layers.
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29. A process for forming a specific reactive element bilayer on surface alloys containing at least 2 wt % of aluminum and at least 2 wt % of titanium with trace amounts of sulfur, the process comprising:
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placing the alloy surface in a sealed environment;
creating an atmosphere of dry atmospheric air and water vapor at an above atmospheric pressure adjacent the surface, the water vapor having a concentration such that a dew point of less than −
25°
C. is achieved;
heating the dry atmospheric air and water vapor to between 550°
C. and 1050°
C.;
reacting oxygen of the water vapor molecules with aluminum metal to form α
-Al2O3 on a surface of the alloy and reacting hydrogen from the water vapor molecules with sulfur to create hydrogen sulfide;
removing hydrogen sulfide from the defined environment;
reducing titanium atoms with aluminum metal and diffusing the reduced titanium atoms outward through the α
-Al2O3 layer and oxidizing the diffused titanium ions to form a Ti2O3 layer and an α
-Al2O3 and Ti2O3 matrix with TiO2 fibers. - View Dependent Claims (30)
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31. A process for forming a specific reactive element bilayer on a substrate containing at least 2 wt % of titanium and at least 2 wt % of aluminum with trace amounts of sulfur, the process comprising:
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(a) placing the alley substrate in a sealed region;
(b) reducing a pressure in the sealed region to achieve a sub-atmospheric partial air pressure between 1×
10−
6 and 1×
10−
2 kPa and a partial water pressure between 1×
10−
6 and 1×
10−
5 kPa at a temperature between 800°
C. and 1050°
C.;
(c) reacting oxygen from water vapor molecules with aluminum metal of the alloy to form α
-Al2O3 and reacting hydrogen from the water vapor molecules with trace sulfur to form hydrogen sulfide;
(d) continuing step (c) to form a crystalline α
-Al2O3 layer of at least 500 Å
at a substrate/barrier layer interface and reducing titanium oxides with aluminum metal to form titanium atoms which diffuse outward through the α
-Al2O3 layer to form a crystalline Ti2O3 layer at a barrier layer/gas interface, which crystalline α
-Al2O3 and crystalline Ti2O3 layers have similar lattice structures;
(e) adjusting a water vapor content of the atmosphere to have a water partial pressure between 1×
10−
3 and 1×
10−
2 kPa at a temperature between 800°
C. and 1050°
C.; and
(f) forming an α
-Al2O3 and Ti2O3 matrix with TiO2 fibers embedded in the matrix.
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32. A method for forming a specific reactive element bilayer on titanium aluminides, the process comprising:
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creating a dry air and water vapor atmosphere with a dew point between −
45°
C. and −
65°
C.;
heating the atmosphere to at least 550°
C.;
reacting oxygen from water vapor molecules in the atmosphere with aluminum in the titanium aluminide, dissociating the water molecules and forming α
-Al2O3 on a surface of the titanium aluminide and reacting hydrogen disassociated from the water vapor molecules with sulfur in the titanium aluminide to remove the sulfur from the titanium aluminide;
reducing titanium in the titanium aluminide by aluminum and diffusing the reduced titanium atoms through the α
-Al2O3 layer and oxidizing the titanium atoms which diffused through the α
-Al2O3 layer to form a Ti2O3 layer;
raising the temperature of the atmosphere to at least 800°
C. and forming an α
-Al2O3 and Ti2O3 matrix and TiO2 fibers in the matrix.
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33. A process for forming a specific reactive element bilayer on a titanium aluminide substrate, the process comprising:
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creating an atmosphere within a vacuum with a partial air pressure between 1×
10−
6 and 1×
10−
2 kPa with a partial water vapor pressure between 1×
10−
6 and 1×
10−
5 kPa at a temperature above 800°
C. contiguous to a surface of the titanium aluminide substrate such that water vapor molecules react with aluminum in the substrate to form an α
-Al2O3 layer on the substrate which is grown to a thickness of at least 500 Å and
forming a Ti2O3 layer on the α
-Al2O3 layer;
adjusting the partial water pressure of the atmosphere to between 1×
10−
3 and 1×
10−
2 kPa at a temperature of at least 800°
C. forming the α
-Al2O3 and Ti2O3 layers into a crystalline α
-Al2O3 and Ti2O3 matrix and TiO2 fibers embedded in the matrix. - View Dependent Claims (34)
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35. A process for forming an α
- -Al2O3 protective oxygen barrier on a surface of a substrate containing aluminum and at least one additional element which does not form oxides in the presence of aluminum, the process comprising;
creating an atmosphere of atmospheric air with below 750 ppm water vapor at a temperature between 550°
C. and 1050°
C.;
reacting water vapor molecules with aluminum in the substrate to form a crystalline α
-Al2O3 layer of at least 500 Å
on the substrate.
- -Al2O3 protective oxygen barrier on a surface of a substrate containing aluminum and at least one additional element which does not form oxides in the presence of aluminum, the process comprising;
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36. A process for forming an α
- -Al2O3 oxide protective oxygen barrier on a surface of a substrate containing at least 2 wt % aluminum and at least one of nickel, iron, and chromium, the process comprising;
(a) creating an atmosphere of atmospheric air and water vapor at sub-atmospheric pressures on a surface of the substrate with a concentration of water vapor between 1×
10−
5 and 1×
10−
6 kPa at a temperature between 550°
C. and 1050°
C.; and
(b) while continuing step (a), reacting oxygen from the water vapor with aluminum to form a crystalline α
-Al2O3 layer on the surface of the substrate and reacting hydrogen reduced from the water vapor with sulfur to remove sulfur from the substrate enabling a stronger bond between the α
-Al2O3 layer and the substrate.
- -Al2O3 oxide protective oxygen barrier on a surface of a substrate containing at least 2 wt % aluminum and at least one of nickel, iron, and chromium, the process comprising;
Specification