Methods of producing deformed metal articles

Abstract

A method of making metal articles as well as sputtering targets is described, which involves deforming an ingot to preferred dimensions. In addition, products made by the process of the present invention are further described.

Description

BRIEF DESCRIPTION OF DRAWINGS

The patent or application file contains at least one drawing executed in color. Copies of this patent or patent application publication with color drawing(s) will be provided by the Office upon request and payment of the necessary fee.

FIGS. 1 a and 1b illustrate a transverse rolling process.

FIG. 2 is a schematic representation of a deformation process according to one embodiment of the present invention.

FIG. 3 is a schematic representation of a deformation process according to one embodiment of the present invention.

FIG. 4 (in color) is an orientation color coded map with an inverse pole figure for a tantalum plate of the present invention.

FIG. 5 (in color) is a crystal direction map with a 5 degree tolerance for a tantalum plate of the present invention.

FIG. 6 (in color) is a crystal direction map with a 10 degree tolerance for a tantalum plate of the present invention.

FIG. 7 (in color) is a crystal direction map with a 15 degree tolerance for a tantalum plate of the present invention.

FIG. 8 (in color) are pole figure plots for (111), (001), and (110), and FIG. 9 (in color) are the inverse pole figure plots for a tantalum plate of the present invention.

FIG. 10 (in color) is a grain size histogram and data for a tantalum plate of the present invention.

FIG. 11 is a flow chart showing various process steps and parameters for various embodiments of the present invention.

FIG. 12 is a drawing of a metal article, such as a disc, which further shows desirable locations to take samples of the metal article to measure texture and/or grain size to gain a full understanding of the metal article throughout on all planes (x,y,z).

Claims

1. A method of making a metal article having a final thickness comprising: deforming a metal ingot to form a rectangular slab having a length, width, and thickness, wherein two of the three dimensions are within 25% of each other,a first rolling of said rectangular slab to form an intermediate plate, wherein said first rolling includes a plurality of rolling passes; anda second rolling of said intermediate plate to form a metal plate, wherein said second rolling includes a plurality of rolling passes, and wherein each of said rolling passes of said second rolling imparts a true strain reduction of from about 0.06 to 0.18 per pass.

2. The method of claim 1, wherein said two of three dimensions are within 15% of each other.

3. The method of claim 1, wherein said two of three dimensions are within 10% of each other.

4. The method of claim 1, wherein said two of three dimensions are within 1% of each other.

5. The method of claim 1, wherein said two of three dimensions are width and thickness.

6. The method of claim 1, wherein said metal ingot has a diameter of at least 9½ inches.

7. The method of claim 1, wherein said metal ingot has a diameter of at least 11 inches.

8. The method of claim 1, wherein said metal ingot has a diameter of from 10 inches to about 20 inches.

9. The method of claim 1, wherein said rectangular slab has a thickness prior to said first rolling that is at least 5 times thicker than the final thickness of said metal article.

10. The method of claim 1, wherein said rectangular slab has a thickness prior to said first rolling that is at least 10 times thicker than the final thickness of said metal article.

11. The method of claim 1, wherein said rectangular slab has a thickness prior to said first rolling that is at least 15 times thicker than the final thickness of said metal article.

12. The method of claim 1, wherein said rectangular slab has a thickness prior to said first rolling that is at least 20 times thicker than the final thickness of said metal article.

13. The method of claim 1, wherein a total true strain reduction imparted by said second rolling is from about 0.10 to about 1.0 of a true strain reduction.

14. The method of claim 1, wherein a total true strain reduction imparted by said second rolling is from about 0.20 to about 0.5 of a true strain reduction.

15. The method of claim 1, wherein said first rolling comprises a rolling schedule defined by changes in mill gap settings.

16. The method of claim 1, wherein a final rolling pass of said second rolling imparts a true strain reduction that is equal to or greater than a true strain reduction imparted by any other rolling pass.

17. The method of claim 1, wherein said metal ingot is niobium, tantalum, or an alloy thereof.

18. The method of claim 1, wherein said metal ingot is copper or titanium or alloys thereof.

19. The method of claim 1, further comprising annealing said slab prior to said first rolling.

20. The method of claim 19, wherein said annealing is under vacuum or inert conditions at a temperature of from about 700° to about 1500° C. for a time of from about 30 minutes to about 24 hours.

21. The method of claim 1, further comprising providing said rectangular slab with two opposing rolling surfaces that are flat to within about 0.02 inches.

22. The method of claim 1, wherein said rectangular slab has a thickness of from about 3 to about 8 inches, a width of from about 3 to about 8 inches, and a length of from about 10 to about 48 inches.

23. The method of claim 1, wherein said intermediate plate has a thickness of from about 0.40 to about 1.5 inches.

24. The method of claim 1, wherein said intermediate plate has a length that is greater than a length of said rectangular slab by about 10% or less.

25. The method of claim 1, further comprising annealing said intermediate plate.

26. The method of claim 25, wherein said annealing is under vacuum or inert conditions at a temperature of from about 700° C. to about 1500° C. for a time of from about 30 minutes to about 24 hours.

27. The method of claim 1, wherein at least one of said rolling passes of said second rolling is in a transverse direction relative to at least one of said rolling passes of said first rolling.

28. The method of claim 1, wherein said rolling passes of said second rolling are multi-directional.

29. The method of claim 1, wherein said metal ingot has a cross-sectional area and said rectangular slab has a cross-sectional area, wherein in forming said regular slab, said cross-sectional area of said metal ingot is subjected to a true strain reduction of at least 95% based on a true strain, compared to cross-sectional area of said rectangular slab.

30. The method of claim 29, wherein said true strain reduction in cross-sectional area is at least 100%.

31. A metal plate formed by the method of claim 1.

32. The metal plate of claim 31 wherein said metal plate has an average grain size of 20 microns or less.

33. A method of making a metal article having a final thickness comprising: a) deforming a metal ingot having a cross-sectional area to form a slab having a cross-sectional area, wherein the cross-sectional area of the slab is at least 95% less based on a total true strain reduction, compared to the cross-sectional area of the metal ingot;b) a first rolling of said slab to form an intermediate plate or a metal plate, wherein said first roiling includes a plurality of rolling passes;c) optionally, a second rolling of said intermediate plate to form a metal plate, wherein said second rolling includes a plurality of rolling passes, and wherein each of said rolling passes of said second rolling imparts a true strain reduction of about 0.06 or more.

34. The method of claim 33, wherein said cross-sectional area of the slab is at least 100% less.

35. The method of claim 33, wherein said cross-sectional area of the slab is from 9% to 500% less.

36. The method of claim 33, wherein said metal ingot has a diameter of at least 9½ inches.

37. The method of claim 33, wherein said metal ingot has a diameter of at least 11 inches.

38. The method of claim 33, wherein said metal ingot has a diameter of from 10 inches to about 20 inches.

39. The method of claim 33, wherein a total true strain reduction imparted by said second rolling is from about 0.10 to about 1.0 of a true strain reduction.

40. The method of claim 33, wherein a total true strain reduction imparted by said second rolling is from about 0.20 to about 0.5 of a true strain reduction.

41. The method of claim 33, wherein said metal ingot is niobium, tantalum, or an alloy thereof.

42. The method of claim 33, further comprising annealing said slab prior to said first rolling.

43. The method of claim 33, further comprising annealing said intermediate plate or said metal plate or both.

44. The method of claim 33, wherein said second rolling occurs and at least one of said rolling passes of said second rolling is in a transverse direction relative to at least one of said rolling passes of said first rolling.

45. A BCC metal having a texture gradient uniformity factor (H) of 0.3 or less.

46. The BCC metal of claim 45, wherein said texture gradient uniformity factor is from about 0.1 to 0.2.

47. The BCC metal of claim 45, wherein said texture gradient uniformity factor is from about 0.12 to about 0.17.

48. A BCC metal having a texture gradient banding factor (B) of 0.1 or less.

49. The BCC metal of claim 48, wherein said texture gradient banding factor is from about 0.01 to about 0.075.

50. The BCC metal of claim 48, wherein said texture gradient banding factor is from about 0.02 to about 0.05.

51. The BCC metal of claim 48, wherein said BCC metal has a texture gradient uniformity factor (H) of 0.2 or less.

52. The BCC metal of claim 48, wherein said texture gradient uniformity factor is from about 0.1 to 0.2.

53. The BCC metal of claim 48, wherein said texture gradient uniformity factor is from about 0.12 to about 0.17.

54. The BCC metal of claim 48, wherein said BCC metal is tantalum.

55. The BCC metal of claim 45, wherein said BCC metal is tantalum.

56. The BCC metal of claim 48, having a metal purity of at least 99.95% of said BCC metal.

57. The BCC metal of claim 48, wherein said BCC metal has an average grain size of about 75 microns or less.

58. The BCC metal of claim 48, wherein said BCC metal is tantalum and has a primary (111) texture throughout the thickness of the BCC metal.

59. The method of claim 33, wherein said second rolling occurs.

60. The method of claim 33, wherein said first rolling is a clock rolling to form said metal plate.

61. The method of claim 1, wherein said true strain reduction is from about 0.06 to 0.15 per pass.

62. The method of claim 1, wherein the subsequent rolling pass in the second rolling is within 25% of the true stain reduction of the previous rolling pass.

63. The method of claim 1, wherein the subsequent rolling pass in the second rolling is within 5% of the true strain reduction of the previous rolling pass.

64. The BCC metal of claim 45, wherein the uniformity factor varies no more than ±0.1 throughout the BCC metal.

65. The BCC metal of claim 48, wherein the texture gradient banding factor varies no more than ±0.05 throughout the BCC metal.