Process for preparing metal powders having low oxygen content, powders so-produced and uses thereof
View Patent ↗The present invention is directed to a process for the preparation of a metal powder having a purity at least as high as the starting powder and having an oxygen content of 10 ppm or less comprising heating said metal powder containing oxygen in the form of an oxide, with the total oxygen content being from 50 to 3000 ppmf in an inert atmosphere at a pressure of from 1 bar to 10 −7 to a temperature at which the oxide of the metal powder becomes thermodynamically unstable and removing the resulting oxygen via volatilization. The metal powder is preferably selected from the group consisting of tantalum, niobium, molybdenum, hafnium, zirconium, titanium, vanadium, rhenium and tungsten. The invention also relates to the powders produced by the process and the use of such powders in a cold spray process.
1. A method of producing low-oxygen metal powder, the method comprising:
heating a metal powder comprising 50 ppm to 3000 ppm oxygen in an inert hydrogen-free atmosphere to a temperature at which an oxide of the metal powder becomes thermodynamically unstable; and
applying a pressure within the range of 10 −7 bar to 1 bar, thereby volatilizing the oxygen and forming a low-oxygen metal powder,
wherein the low-oxygen metal powder has an oxygen content of 10 ppm or less and a purity at least as high as a purity of the metal powder.
2. The method of claim 1 , wherein the metal powder is selected from the group consisting of tantalum, niobium, molybdenum, hafnium, zirconium, titanium, vanadium, rhenium, and tungsten.
3. The method of claim 1 , wherein the inert atmosphere comprises at least one of argon, helium, neon, krypton, or xenon.
4. The method of claim 1 , wherein the low-oxygen metal powder has a hydrogen content of 1 ppm or less, a magnesium content of 1 ppm or less, and an alkali metal content of 1 ppm or less.
5. The method of claim 1 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.
6. The method of claim 1 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.
7. The method of claim 1 , wherein the inert hydrogen-free atmosphere is substantially free of magnesium.
8. The method of claim 1 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder without passivating the low-oxygen metal powder therebetween.
9. The method of claim 8 , wherein spray depositing comprises cold spray.
10. A method of producing low-oxygen tantalum powder, the method comprising:
heating a tantalum powder comprising 50 ppm to 3000 ppm oxygen to a temperature at which an oxide of the tantalum powder becomes thermodynamically unstable; and
applying a pressure within the range of 10 −7 bar to 1 bar, thereby volatilizing the oxygen and forming a low-oxygen tantalum powder,
wherein the low-oxygen tantalum powder has an oxygen content of 10 ppm or less and a purity at least as high as a purity of the tantalum powder.
11. The method of claim 10 , wherein heating the tantalum powder comprises gas-plasma heating, induction heating, or resistance heating.
12. The method of claim 10 , wherein a surface area of the low-oxygen tantalum powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.
13. The method of claim 10 , wherein the tantalum powder is heated in an ambient substantially free of magnesium.
14. The method of claim 10 , further comprising, after forming the low-oxygen tantalum powder, spray depositing the low-oxygen tantalum powder without passivating the low-oxygen tantalum powder therebetween.
15. The method of claim 14 , wherein spray depositing comprises cold spray.
16. A method of producing low-oxygen metal powder, the method comprising:
heating a metal powder comprising 50 ppm to 3000 ppm oxygen to a temperature at which an oxide of the metal powder becomes thermodynamically unstable, the metal powder being selected from the group consisting of tantalum, niobium, molybdenum, hafnium, zirconium, titanium, vanadium, rhenium, and tungsten; and
applying a pressure within the range of 10 −7 bar to 1 bar, thereby volatilizing the oxygen and forming a low-oxygen metal powder,
wherein the low-oxygen metal powder has an oxygen content of 10 ppm or less, a purity at least as high as a purity of the metal powder, a hydrogen content of 1 ppm or less, a magnesium content of 1 ppm or less, and an alkali metal content of 1 ppm or less.
17. The method of claim 16 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.
18. The method of claim 16 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.
19. The method of claim 16 , wherein the metal powder is heated in an ambient substantially free of magnesium.
20. The method of claim 16 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder without passivating the low-oxygen metal powder therebetween.
21. The method of claim 20 , wherein spray depositing comprises cold spray.
22. A method of producing low-oxygen metal powder, the method comprising:
heating a metal powder comprising 50 ppm to 3000 ppm oxygen to a temperature at which an oxide of the metal powder becomes thermodynamically unstable but below a melting point of the metal powder; and
applying a pressure within the range of 10 −7 bar to 1 bar, thereby volatilizing the oxygen and forming a low-oxygen metal powder,
wherein the low-oxygen metal powder has an oxygen content of 10 ppm or less and a purity at least as high as a purity of the metal powder.
23. The method of claim 22 , wherein the metal powder is heated in an inert atmosphere substantially free of hydrogen and magnesium.
24. The method of claim 22 , wherein the metal powder is selected from the group consisting of tantalum, niobium, molybdenum, hafnium, zirconium, titanium, vanadium, rhenium, and tungsten.
25. The method of claim 23 , wherein the inert atmosphere comprises at least one of argon, helium, neon, krypton, or xenon.
26. The method of claim 22 , wherein the low-oxygen metal powder has a hydrogen content of 1 ppm or less, a magnesium content of 1 ppm or less, and an alkali metal content of 1 ppm or less.
27. The method of claim 22 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.
28. The method of claim 22 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.
29. The method of claim 22 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder without passivating the low-oxygen metal powder therebetween.
30. The method of claim 29 , wherein spray depositing comprises cold spray.