Process for producing tantalum alloys

Patent metadata

Field	Value
Publication number	US-9260765-B2
Application number	US-201313844457-A
Country	US
Kind code	B2
Filing date	Mar 15, 2013
Priority date	Mar 15, 2013
Publication date	Feb 16, 2016
Grant date	Feb 16, 2016

Abstract

Processes for the production of tantalum alloys are disclosed. The processes use aluminothermic reactions to reduce tantalum pentoxide to tantalum metal.

First claim

What is claimed is:

1. A process for the production of a tantalum alloy comprising:
forming a reactant mixture comprising:
tantalum pentoxide powder;
iron (III) oxide powder;
copper (II) oxide powder;
barium peroxide powder;
aluminum metal powder; and
tungsten metal powder;

positioning a magnesium oxide powder layer on at least a bottom surface of a graphite reaction vessel;
positioning the reactant mixture in the graphite reaction vessel on top of the magnesium oxide powder layer;
positioning a tantalum or tantalum alloy ignition wire in contact with the reactant mixture;
sealing the reaction vessel inside a reaction chamber;
establishing a vacuum inside the reaction chamber;
energizing the ignition wire to initiate aluminothermic reactions between components of the reactant mixture, thereby producing reaction products comprising:
a monolithic and fully-consolidated alloy regulus comprising tantalum and tungsten; and
a separate slag phase comprising aluminum oxide and barium oxide;

cooling the reaction products to ambient temperature;
removing the reaction products from the reaction vessel; and
separating the slag and the regulus.

2. The process of claim 1 , wherein the regulus comprises a tantalum yield of at least 90%, on a metal weight basis, of initial tantalum provided by the tantalum pentoxide reactant.

3. The process of claim 1 , wherein the regulus comprises a tantalum yield of at least 93%, on a metal weight basis, of initial tantalum provided by the tantalum pentoxide reactant.

4. The process of claim 1 , wherein the regulus comprises at least 1.0% tungsten based on total weight of the regulus.

5. The process of claim 1 , wherein the regulus comprises at least 80% tantalum based on total weight of the regulus.

6. The process of claim 1 , wherein the reactant mixture comprises, based on total weight of the reactant mixture:
55.1% to 57.1% tantalum pentoxide powder;
2.0% to 3.5% iron (III) oxide powder;
1.7% to 3.2% copper (II) oxide powder;
21.5% to 23.5% barium peroxide powder;
14.7% to 16.7% aluminum metal powder; and
0.5% to 15% tungsten metal powder.

7. The process of claim 1 , further comprising electron beam melting the regulus.

8. A process for the production of a tantalum alloy comprising:
positioning a reactant mixture in a reaction vessel, the reactant mixture comprising:
tantalum pentoxide powder;
at least one of iron (III) oxide powder and copper (II) oxide powder;
barium peroxide powder;
aluminum metal powder; and
at least one of niobium pentoxide powder, tungsten metal powder, and tungsten trioxide powder; and

initiating aluminothermic reactions between components of the reactant mixture.

9. The process of claim 8 , wherein the reactant mixture comprises:
tantalum pentoxide powder;
iron (III) oxide powder;
copper (II) oxide powder;
barium peroxide powder;
aluminum metal powder; and
tungsten metal powder.

10. The process of claim 9 , wherein the reactant mixture comprises, based on total weight of the reactant mixture:
55.1% to 57.1% tantalum pentoxide powder;
2.0% to 3.5% iron (III) oxide powder;
1.7% to 3.2% copper (II) oxide powder;
21.5% to 23.5% barium peroxide powder;
14.7% to 16.7% aluminum metal powder; and
0.5% to 15% tungsten metal powder.

11. The process of claim 8 , wherein the reactant mixture comprises:
tantalum pentoxide powder;
niobium pentoxide powder
iron (III) oxide powder;
copper (II) oxide powder;
barium peroxide powder; and
aluminum metal powder.

12. The process of claim 8 , wherein the reaction vessel comprises a graphite bottom surface.

13. The process of claim 8 , wherein the reaction vessel comprises a graphite sidewall.

14. The process of claim 8 , wherein a layer of magnesium oxide is positioned on at least a bottom surface of the reaction vessel.

15. The process of claim 14 , wherein the layer of magnesium oxide comprises at least one of:
a layer of magnesium oxide powder;
a thermally-sprayed magnesium oxide coating layer;
a painted magnesium oxide coating layer; or
a magnesium oxide sheet or wallboard positioned immediately adjacent to the bottom surface of the reaction vessel.

16. The process of claim 8 , wherein initiating the aluminothermic reactions between the reactant mixture components comprises energizing an ignition wire positioned in contact with the reactant mixture.

17. The process of claim 16 , wherein the ignition wire is one of:
submerged in the reactant mixture in the reaction vessel; or
positioned in a starter bag positioned on top of the reactant mixture in the reaction vessel, wherein the starter bag further contains powder comprising:
aluminum metal powder; and
a second powder selected from the group consisting of tantalum pentoxide powder, niobium pentoxide powder, iron (III) oxide powder, copper (II) oxide powder, barium peroxide powder, and combinations of any thereof.

18. The process of claim 16 , wherein energizing the ignition wire comprises sending a current of at least 60 amps through the ignition wire for at least 1 second.

19. The process of claim 8 , before initiating the aluminothermic reactions, further comprising sealing the reaction vessel inside a reaction chamber and establishing a vacuum inside the reaction chamber.

20. The process of claim 8 , wherein the aluminothermic reactions produce reaction products comprising:
a monolithic and fully-consolidated alloy regulus comprising tantalum and one of tungsten or niobium; and
a separate slag phase comprising aluminum oxide and barium oxide.

21. The process of claim 20 , further comprising cooling the reaction products to ambient temperature; removing the reaction products from the reaction vessel; and separating the slag and the regulus.

22. The process of claim 20 , wherein the regulus comprises a tantalum yield of at least 90%, on a metal weight basis, of initial tantalum provided by the tantalum pentoxide reactant.

23. The process of claim 20 , wherein the regulus comprises a tantalum yield of at least 93%, on a metal weight basis, of initial tantalum provided by the tantalum pentoxide reactant.

24. The process of claim 20 , wherein the regulus comprises at least 1.0% tungsten based on total weight of the regulus.

25. The process of claim 20 , wherein the regulus comprises at least 80% tantalum based on total weight of the regulus.

26. The process of claim 20 , further comprising electron beam melting the regulus.

27. A process for the production of a tantalum alloy comprising:
conducting aluminothermic reactions using a reactant mixture comprising:
tantalum pentoxide powder;
at least one of iron (III) oxide powder and copper (II) oxide powder;
barium peroxide powder;
aluminum metal powder; and
at least one of niobium pentoxide powder, tungsten metal powder, and tungsten trioxide powder.

28. The process of claim 27 , wherein the reactant mixture comprises:
tantalum pentoxide powder;
iron (III) oxide powder;
copper (II) oxide powder;
barium peroxide powder;
aluminum metal powder; and
tungsten metal powder.

29. The process of claim 27 , wherein the reactant mixture comprises, based on total weight of the reactant mixture:
55.1% to 57.1% tantalum pentoxide powder;
2.0% to 3.5% iron (III) oxide powder;
1.7% to 3.2% copper (II) oxide powder;
21.5% to 23.5% barium p

Assignees

• Ati Properties Inc

Inventors

• Fajardo Arnel M
• Foltz Iv John W

Classifications

• B22F3/23 Primary

  involving a self-propagating high-temperature synthesis or reaction sintering step {(making cermets by reaction sintering C22C1/051)} · CPC title

• C22C1/045

  Alloys based on refractory metals · CPC title

• C22B34/24

  Obtaining niobium or tantalum · CPC title

• C22C27/02

  Alloys based on vanadium, niobium, or tantalum · CPC title

• C22C1/02

  by melting {(C22C1/1036 takes precedence)} · CPC title