High purity tantalum, products containing the same, and methods of making the same
View Patent ↗High purity tantalum metals and alloys containing the same are described. The tantalum metal preferably has a purity of at least 99.995% and more preferably at least 99.999%. In addition, tantalum metal and alloys thereof are described, which either have a grain size of about 50 microns or less, or a texture in which a (100) intensity within any 5% increment of thickness is less than about 15 random, or an incremental log ratio of (111):(100) intensity of greater than about −4.0, or any combination of these properties. Also described are articles and components made from the tantalum metal which include, but are not limited to, sputtering targets, capacitor cans, resistive film layers, wire, and the like. Also disclosed is a process for making the high purity metal which includes the step of reacting a salt-containing tantalum with at least one compound capable of reducing this salt to tantalum powder and a second salt in a reaction container. The reaction container or liner in the reaction container and the agitator or liner on the agitator are made from a metal material having the same or higher vapor pressure of melted tantalum. The high purity tantalum preferably has a fine and uniform microstructure.
1. A process of making a sputtering component from tantalum metal, comprising:
a) mechanically or chemically clean surfaces of the tantalum metal, wherein the tantalum metal has a sufficient starting cross-sectional area to permit steps b) through g);
b) flat forging the tantalum metal into at least one rolling slab, wherein the at least one rolling slab has sufficient deformation to achieve substantially uniform recrystallization after annealing in step d);
c) mechanically or chemically clean surfaces of the at least one rolling slab;
d) annealing the at least one rolling slab at a sufficient temperature and for a sufficient time to achieve at least partial recrystallization of the at least one rolling slab;
e) cold or warm rolling the at least one rolling slab in both the perpendicular and parallel directions to the axis of the starting tantalum metal to form at least one plate;
f) flattening the at least one plate; and
g) annealing the at least one plate to have an average grain size equal to or less than about 150 microns and a texture substantially void of (100) textural bands;
2. The process of claim 1 , wherein said tantalum sputtering component is a sputtering target.
3. The process of claim 2 , further comprising attaching a backing plate to said sputtering target.
4. The process of claim 2 , wherein said tantalum metal has a purity of at least 99.99% Ta.
5. The process of claim 1 , wherein the tantalum metal has a purity of at least 99.50%.
6. The process of claim 1 , wherein the flat forging occurs after the tantaluml metal is placed in air for at least about 4 hours and from temperatures ranging from ambient to about 1200° C.
7. The process of claim 1 , wherein the cold rolling is transverse rolling at ambient temperatures and the warm rolling is at temperatures of less than about 370° C.
8. The process of claim 1 , wherein the annealing of the plate is vacuum annealing at a temperature and for a time sufficient to achieve recrystallization of the tantalum metal.
9. The process of claim 1 , wherein said tantalum metal is an ingot.
10. The process of claim 1 , wherein said tantalum metal is a 12 inch nominal diameter ingot.
11. The process of claim 1 , wherein the tantalum metal has a purity of at least 99.99% Ta.
12. The process of claim 1 , wherein said tantalum sputtering component has an average grain size of about 125 microns or less.
13. The process of claim 1 , wherein said tantalum sputtering component has an average grain size of 50 microns or less.
14. The process of claim 1 , wherein said tantalum sputtering component is fully recrystallized.
15. The process of claim 1 , wherein about 80% or more of said tantalum sputtering component is recrystallized.
16. A process of making a sputtering component from tantalum metal, comprising:
a) mechanically or chemically clean surfaces of the tantalum metal, wherein the tantalum metal has a sufficient starting cross-sectional area to permit steps b) through I);
b) round forging the tantalum metal into at least one rod, wherein the at least one rod has sufficient deformation to achieve substantially uniform recrystallization after annealing in step d) or step f);
c) cutting the rod into billets and mechanically or chemically clean the surfaces of the billets;
d) optionally annealing the billets to achieve at least partial recrystallization;
e) axially forging billets into preforms;
f) optionally annealing the preforms to achieve at least partial recrystallization;
g) cold rolling the performs into at least one plate; and
h) optionally mechanically or chemically clean the surfaces of the at least one plate; and
i) annealing the at least one plate to have an average grain size equal to or less than about 150 microns and a texture substantially void of (100) textural bands, wherein annealing occurs at least in step d) or f) or both.
17. The process of claim 16 , wherein said tantalum sputtering component is a sputtering target.
18. The process of claim 16 , wherein the tantalum has a purity of at least 99.50%.
19. The process of claim 16 , wherein the round forging occurs after subjecting the tantalum metal to temperatures of about 370° C. or lower.
20. The process of claim 16 , wherein prior to forging the billets, the billets are annealed.
21. The process of claim 16 , wherein prior to cold rolling of the preforms, the preforms are annealed.
22. The process of claim 16 , wherein the annealing of the preforms is vacuum annealing at a sufficient temperature and for a time to achieve recrystallization.
23. The process of claim 16 , wherein said tantalum metal is an ingot.
24. The process of claim 16 , wherein said tantalum metal is a 12 inch nominal diameter ingot
25. The process of claim 16 , wherein said tantalum metal has a purity of at least 99.99% Ta.
26. The process of claim 16 , further comprising attaching a backing plate to said sputtering target.
27. The process of claim 16 , wherein said tantalum sputtering component has an average grain size of about 125 microns or less.
28. The process of claim 16 , wherein said tantalum sputtering component has an average grain size of 50 microns or less.
29. The process of claim 16 , wherein said tantalum sputtering component is fully recrystallized.
30. The process of claim 16 , wherein about 80% or more of said tantalum sputtering component is recrystallized.