IP Library Granted Patent US 8,715,386
Granted Patent B2
US 8,715,386 · App. 13/529,148 · Granted May 6, 2014

Process for preparing metal powders having low oxygen content, powders so-produced and uses thereof

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Quick Facts
Patent No.
US 8,715,386
App. No.
13/529,148
Granted
May 6, 2014
Kind
B2
Abstract

In various embodiments, low-oxygen metal powder is produced by heating a metal powder to a temperature at which an oxide of the metal powder becomes thermodynamically unstable and applying a pressure to volatilize the oxygen.

Claims (69)

1. 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

thereduring, applying a pressure within the range of 10 −7 bar to 10 −3 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.

2. The method of claim 1 , wherein the metal powder is heated in a hydrogen-free atmosphere.

3. The method of claim 1 , wherein the metal powder is heated in an atmosphere comprising at least one of argon, helium, neon, krypton, or xenon.

4. The method of claim 1 , wherein the metal powder is heated in an atmosphere substantially free of magnesium.

5. 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.

6. The method of claim 1 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.

7. 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.

8. The method of claim 1 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder.

9. The method of claim 8 , wherein the low-oxygen metal powder is spray deposited after formation without passivating the low-oxygen metal powder therebetween.

10. The method of claim 8 , wherein spray depositing comprises cold spray.

11. The method of claim 1 , wherein the metal powder is tungsten and the oxygen content of the low-oxygen metal powder is 5 ppm or less.

12. A method of producing low-oxygen metal powder, the method comprising:

heating a metal powder comprising 50 ppm to 3000 ppm oxygen in a 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.

13. The method of claim 12 , wherein the metal powder is selected from the group consisting of tantalum, niobium, molybdenum, hafnium, zirconium, titanium, vanadium, rhenium, and tungsten.

14. The method of claim 12 , wherein the hydrogen-free atmosphere comprises at least one of argon, helium, neon, krypton, or xenon.

15. The method of claim 12 , wherein the hydrogen-free atmosphere is substantially free of magnesium.

16. The method of claim 12 , 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.

17. The method of claim 12 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.

18. The method of claim 12 , 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 12 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder.

20. The method of claim 19 , wherein the low-oxygen metal powder is spray deposited after formation without passivating the low-oxygen metal powder therebetween.

21. The method of claim 19 , wherein spray depositing comprises cold spray.

22. The method of claim 12 , wherein the metal powder is tungsten and the oxygen content of the low-oxygen metal powder is 5 ppm or less.

23. 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; 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 hydrogen content of 1 ppm or less.

24. The method of claim 23 , 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 metal powder is heated in a hydrogen-free atmosphere.

26. The method of claim 23 , wherein the metal powder is heated in an atmosphere comprising at least one of argon, helium, neon, krypton, or xenon.

27. The method of claim 23 , wherein the metal powder is heated in an atmosphere substantially free of magnesium.

28. The method of claim 23 , wherein the low-oxygen metal powder has a magnesium content of 1 ppm or less and an alkali metal content of 1 ppm or less.

29. The method of claim 23 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.

30. The method of claim 23 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.

31. The method of claim 23 , wherein the pressure is within the range of 10 −7 bar to 10 −3 bar.

32. The method of claim 23 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder.

33. The method of claim 32 , wherein the low-oxygen metal powder is spray deposited after formation without passivating the low-oxygen metal powder therebetween.

34. The method of claim 32 , wherein spray depositing comprises cold spray.

35. The method of claim 23 , wherein the metal powder is tungsten and the oxygen content of the low-oxygen metal powder is 5 ppm or less.

36. A method of producing low-oxygen metal powder, the method comprising:

heating a metal powder comprising 50 ppm to 3000 ppm oxygen in a hydrogen-free atmosphere to a temperature at which an oxide of the metal powder becomes thermodynamically unstable; and

thereduring, applying a pressure within the range of 10 −7 bar to 10 −3 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.

37. The method of claim 36 , wherein the metal powder is heated in an atmosphere comprising at least one of argon, helium, neon, krypton, or xenon.

38. The method of claim 36 , wherein the metal powder is heated in an atmosphere substantially free of magnesium.

39. The method of claim 36 , 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.

40. The method of claim 36 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.

41. The method of claim 36 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.

42. The method of claim 36 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder.

43. The method of claim 42 , wherein the low-oxygen metal powder is spray deposited after formation without passivating the low-oxygen metal powder therebetween.

44. The method of claim 42 , wherein spray depositing comprises cold spray.

45. The method of claim 36 , wherein the metal powder is tungsten and the oxygen content of the low-oxygen metal powder is 5 ppm or less.

46. 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; and

thereduring, applying a pressure within the range of 10 −7 bar to 10 −3 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 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.

47. The method of claim 46 , wherein the metal powder is heated in an atmosphere comprising at least one of argon, helium, neon, krypton, or xenon.

48. The method of claim 46 , wherein the metal powder is heated in an atmosphere substantially free of magnesium.

49. The method of claim 46 , wherein heating the metal powder comprises gas-plasma heating, induction heating, or resistance heating.

50. The method of claim 46 , wherein a surface area of the low-oxygen metal powder ranges from approximately 100 cm 2 /g to approximately 10,000 cm 2 /g.

51. The method of claim 46 , further comprising, after forming the low-oxygen metal powder, spray depositing the low-oxygen metal powder.

52. The method of claim 51 , wherein the low-oxygen metal powder is spray deposited after formation without passivating the low-oxygen metal powder therebetween.

53. The method of claim 51 , wherein spray depositing comprises cold spray.

54. The method of claim 46 , wherein the metal powder is tungsten and the oxygen content of the low-oxygen metal powder is 5 ppm or less.

Assignments (7)
CHANGE OF NAME Recorded Apr 5, 2022
From: H.C. STARCK INC.
To: MATERION NEWTON INC.
Reel/Frame 059596/0925 →
RELEASE OF SECURITY INTEREST Recorded Nov 2, 2021
From: GLAS TRUST CORPORATION LIMITED
To: H.C. STARCK INC.
Reel/Frame 058768/0827 →
RELEASE OF SECURITY INTEREST Recorded Nov 2, 2021
From: GLAS TRUST CORPORATION LIMITED
To: H.C. STARCK INC.
Reel/Frame 058769/0242 →
SECURITY INTEREST Recorded Nov 1, 2021
From: H.C. STARCK INC.
To: JPMORGAN CHASE BANK, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 057978/0970 →
SECURITY INTEREST Recorded Mar 31, 2016
From: H.C. STARCK INC.
To: GLAS TRUST CORPORATION LIMITED, AS SECURITY AGENT FOR THE BENEFIT OF THE SENIOR SECURED PARTIES
Reel/Frame 038311/0460 →
SECURITY INTEREST Recorded Mar 31, 2016
From: H.C. STARCK INC.
To: GLAS TRUST CORPORATION LIMITED, AS SECURITY AGENT FOR THE BENEFIT OF THE SECOND LIEN SECURED PARTIES
Reel/Frame 038311/0472 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 11, 2013
From: WU, RONG-CHEIN R.; HAYWISER, LEAH F.; SHEKHTER, LEONID N.; MILLER, STEVEN A.
To: H.C. STARCK INC.
Reel/Frame 031760/0562 →