Refractory metal plates
A refractory metal plate is provided. The plate has a center, a thickness, an edge, a top surface and a bottom surface, and has a crystallographic texture (as characterized by through, thickness gradient, banding severity; and variation across the plate, for each of the texture components 100//ND and 111//ND, which is substantially uniform throughout the plate.
1. A method of forming a refractory metal plate, the method comprising:
(A) providing a refractory metal ingot;
(B) cleaning the ingot;
(C) cutting the ingot to produce a workpiece therefrom;
(D) performing a plurality of process cycles, each process cycle comprising (i) upset forging the workpiece, (ii) forging back the workpiece after upset forging the workpiece, and (iii) annealing the workpiece before or after forging back the workpiece;
(E) cutting the workpiece to produce a plate therefrom;
(F) asymmetrically rolling the plate one or more times at an angle of incline between 2° and 20° relative to horizontal; and
(G) annealing the rolled plate to achieve substantially full recrystallization.
2. The method of claim 1 , further comprising, between steps (D) and (E):
upset forging the workpiece, the workpiece having a first diameter;
forging back the workpiece to a second diameter less than the first diameter;
annealing the workpiece; and
forging back the workpiece to a third diameter less than the second diameter.
3. The method of claim 1 , wherein the angle of incline is between 3° and 7°.
4. The method of claim 1 , wherein the plate is asymmetrically rolled a plurality of times during step (F).
5. The method of claim 4 , wherein the plate is rotated at a predetermined angle about a vertical axis between rolling passes.
6. The method of claim 4 , wherein the plate is flipped between rolling passes.
7. The method of claim 1 , further comprising, after step (G), bonding the plate to a backing plate.
8. The method of claim 1 , wherein, after step (G):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement;
an average through-thickness gradient is less than or equal to 6% per mm for 111//ND; and
a maximum through-thickness gradient is less than or equal to 13% per mm for 111//ND.
9. The method of claim 1 , wherein, after step (G):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement; and
an average banding severity is less than or equal to 6% per mm for 111//ND.
10. The method of claim 1 , wherein, after step (G):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement; and
a maximum banding severity is less than or equal to 8% per mm for 111//ND.
11. A method of forming a refractory metal plate, the method comprising:
(A) cold isostatically pressing a refractory metal powder to a density of 60%-90% to form a preform;
(B) hot isostatically pressing the preform to a density of approximately 100% to form a billet;
(C) annealing the billet;
(D) cutting the billet to produce a plate therefrom;
(E) asymmetrically rolling the plate one or more times at an angle of incline between 2° and 20° relative to horizontal; and
(F) annealing the rolled plate to achieve substantially full recrystallization.
12. The method of claim 11 , wherein the angle of incline is between 3° and 7°.
13. The method of claim 11 , wherein the plate is asymmetrically rolled a plurality of times during step (E).
14. The method of claim 13 , wherein the plate is rotated at a predetermined angle about a vertical axis between rolling passes.
15. The method of claim 13 , wherein the plate is flipped between rolling passes.
16. The method of claim 11 , further comprising, after step (F), bonding the plate to a backing plate.
17. The method of claim 11 , wherein, after step (F):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement;
an average through-thickness gradient is less than or equal to 6% per mm for 111//ND; and
a maximum through-thickness gradient is less than or equal to 13% per mm for 111//ND.
18. The method of claim 11 , wherein, after step (F):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement; and
an average banding severity is less than or equal to 6% per mm for 111//ND.
19. The method of claim 11 , wherein, after step (F):
the plate has a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement; and
a maximum banding severity is less than or equal to 8% per mm for 111//ND.
20. A method of forming a thin film, the method comprising:
providing a refractory metal plate having a center, a thickness, an edge, a top surface, and a bottom surface, the refractory metal plate having a crystallographic texture as characterized by through thickness gradient, banding severity, and variation across the plate for at least one of the texture components 100//ND or 111//ND, using electron back-scatter diffraction with a 15 μm step in both the horizontal and vertical directions for each measurement, wherein (i) an average through-thickness gradient is less than or equal to 6% per mm for 111//ND, and (ii) a maximum through-thickness gradient is less than or equal to 13% per mm for 111//ND;
providing a substrate; and
sputtering the plate to form a film on the substrate, the film comprising the refractory metal.