Methods for fabricating refractory complex concentrated alloys and composites containing such alloys, and bodies containing the same

Patent metadata

Field	Value
Publication number	US-11745259-B2
Application number	US-202117208424-A
Country	US
Kind code	B2
Filing date	Mar 22, 2021
Priority date	Mar 25, 2020
Publication date	Sep 5, 2023
Grant date	Sep 5, 2023

Abstract

Methods for producing final bodies that contain a fine-grained refractory complex concentrated alloy (RCCA), as well as RCCAs, intermediate materials and final bodies containing the RCCAs, and high-temperature devices formed by such final bodies. Such a method includes providing a precursor with one or more precursor compounds containing elements of an RCCA, reducing the precursor compounds in the precursor via reaction with a reducing agent so as to generate the RCCA and a compound comprising a product of the reaction between the reducing agent and the precursor compounds, generating a solid material that contains at least the RCCA, forming with the solid material a porous intermediate body, and consolidating the porous intermediate body so as to partially or completely remove the pore volume from the porous intermediate body, and in doing so yield either a denser final body or a denser film.

First claim

The invention claimed is:

1. A method for producing a final body comprising a fine-grained refractory complex concentrated alloy, wherein the fine-grained refractory complex concentrated alloy has an average grain size of 20 micrometers or less, the method comprising:
providing a precursor comprising one or more precursor compounds containing elements of the fine-grained refractory complex concentrated alloy;
reducing the one or more precursor compounds in the precursor via reaction with a reducing agent to generate the fine-grained refractory complex concentrated alloy and a compound comprising a product of the reaction between the reducing agent and the one or more precursor compounds;
generating a solid material that contains at least the fine-grained refractory complex concentrated alloy;
forming with the solid material a porous intermediate body comprising a pore volume; and
consolidating the porous intermediate body to partially or completely remove the pore volume from the porous intermediate body to yield with the porous intermediate body a film that is on a surface of the final body and has a lower porosity than the porous intermediate body, wherein:
the precursor is a precursor film;
the solid material generated by reducing the one or more precursor compounds in the precursor film is a fine-grained film; and
the porous intermediate body is an intermediate film formed with the fine-grained film.

2. The method of claim 1 , further comprising producing the precursor by:
polymerizing a liquid precursor solution to yield a polymerized precursor; and
pyrolysis of the polymerized precursor to yield the precursor comprising one or more precursor compounds.

3. The method of claim 1 , wherein the elements of the fine-grained refractory complex concentrated alloy comprise two or more of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, and aluminum.

4. The method of claim 1 , wherein the one or more precursor compounds are selected from the group consisting of oxides, nitrides, sulfides, chlorides, fluorides, and mixtures thereof.

5. The method of claim 1 , wherein the reducing agent is selected from the group consisting of one or more of magnesium, calcium, strontium, barium, lithium, sodium, and potassium.

6. The method of claim 1 , wherein the porous intermediate body is consolidated by a process selected from the group consisting of sintering, hot pressing, spark plasma sintering, and hot isostatic pressing.

7. The method of claim 1 , wherein the fine-grained refractory complex concentrated alloy of the final body has an average grain size of 1 micrometer or less.

8. The method of claim 1 , wherein the fine-grained refractory complex concentrated alloy possesses an enhanced mechanical property at a temperature relative to a refractory complex concentrated alloy of the same overall composition that possesses an average grain size that is coarser than the fine-grained refractory complex concentrated alloy, wherein the enhanced mechanical property comprises at least one of higher elastic modulus, higher yield strength, higher ultimate tensile strength, higher ductility, higher toughness, higher creep resistance, higher creep rupture life, higher fatigue strength, enhanced stiffness, and reduced ductile-to-brittle transition temperature.

9. The method of claim 8 , wherein the temperature is greater than 800° C.

10. The method of claim 1 , wherein the fine-grained refractory complex concentrated alloy possesses greater resistance to reaction with a reactive fluid at a temperature relative to a refractory complex concentrated alloy of the same overall composition that possesses an average grain size that is coarser than the fine-grained refractory complex concentrated alloy, wherein the reactive fluid comprises at least one of an oxygen-bearing fluid, a nitrogen-bearing fluid, a sulfur-bearing fluid, a carbon-bearing fluid, a chlorine-bearing fluid, and a fluorine-bearing fluid.

11. The method of claim 10 , wherein the reactive fluid is selected from the group consisting of oxygen-bearing fluids, nitrogen-bearing fluids, sulfur-bearing fluids, carbon-bearing fluids, chlorine-bearing fluids, and fluorine-bearing fluids.

12. The method of claim 10 , wherein the temperature is greater than 800° C.

13. The method of claim 1 , wherein the generating of the solid material comprises removing the compound so that the solid material, the porous intermediate body, and the film do not contain the compound.

14. The method of claim 13 , wherein the compound is removed from the solid material by a process selected from the group consisting of selective dissolution in a fluid, selective reaction with a fluid, and selective segregation in a fluid.

15. The method of claim 13 , wherein the final body is a high-temperature device.

16. The method of claim 15 , wherein the high-temperature device is selected from the group consisting of a high-temperature device for a hypersonic missile, a high-temperature device for a supersonic missile, a high-temperature device for a subsonic missile, a high-temperature device for a hypersonic aircraft, a high-temperature device for a supersonic aircraft, a high-temperature device for a subsonic aircraft, a high-temperature device for a jet engine for aircraft, a high-temperature device for land-based vehicles, a high-temperature device for tanks and other land-based military vehicles, a high-temperature device for surface ships, a high-temperature device for surface military ships and submarines, a high-temperature device for energy production, a high-temperature device used for transportation, a high-temperature device used for manufacturing, a leading edge for a hypersonic missile, a leading edge for a supersonic missile, a leading edge for a hypersonic aircraft, a leading edge for a supersonic aircraft, a leading edge for a hypersonic spacecraft, a leading edge for a supersonic spacecraft, a rocket nozzle, a turbine blade, a piston, a pump impeller, a heat exchanger, a machining tool, and a friction stir welding tool.

17. The method of claim 1 , wherein the solid material is generated to also contain the compound, the porous intermediate body formed from the solid material contains a composite comprising the fine-grained refractory complex concentrated alloy and the compound, and the film consolidated from the porous intermediate body contains the composite.

18. The method of claim 17 , wherein the compound is selected from the group consisting of oxides, nitrides, sulfides, chlorides, and fluorides.

19. The method of claim 17 , wherein the compound is selected from the group consisting of magnesium oxide, calcium oxide, strontium oxide, barium oxide, lithium oxide, sodium oxide, and potassium oxide.

20. The method of claim 17 , wherein the compound has an average grain size of 20 micrometers or less.

21. The method of claim 17 , wherein the compound has an average grain size of 1 micrometer or less.

22. The method of claim 17 , wherein the final body is a high-temperature device.

23. The method of claim 22 , wherein the high-temperature device is selected from the group consisting of a high-temperature device for a hypersonic missile, a high-temperature device for a supersonic missile, a high-temperature device for a subsonic missile, a high-temperature device for a hypersonic aircraft, a high-temperature device for a supersonic aircraft, a high-temperature device for a subsonic aircraft, a high-temper

Assignees

• Purdue Research Foundation

Inventors

• Sandhage Kenneth Henry

Classifications

• B32B15/04

  comprising metal as the main or only constituent of a layer, {which is} next to another layer of {the same or of} a {different material (next to a bituminous or tarry layer B32B11/08; next to a water-setting substance layer B32B13/06; next to a glass layer B32B17/061; next to a cellulosic plastic layer B32B23/042)} · CPC title

• B22F3/001 Primary

  Starting from powder comprising reducible metal compounds (making ferrous alloys starting from compounds C22C33/0235) · CPC title

• B22F3/1143

  involving an oxidation, reduction or reaction step · CPC title

• B22F3/14

  simultaneously · CPC title

• B22F3/16

  in successive or repeated steps · CPC title