IP Library Granted Patent US 9,334,565
Granted Patent B2
US 9,334,565 · App. 13/793,043 · Granted May 10, 2016

Multi-block sputtering target with interface portions and associated methods and articles

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Quick Facts
Patent No.
US 9,334,565
App. No.
13/793,043
Granted
May 10, 2016
Kind
B2
Abstract

A sputtering target that includes at least two consolidated blocks, each block including an alloy including a first metal (e.g., a refractory metal such as molybdenum in an amount greater than about 30 percent by weight) and at least one additional alloying ingredient; and a joint between the at least two consolidated blocks, the joint being prepared free of any microstructure derived from a diffusion bond of an added loose powder. A process for making the target includes hot isostatically pressing (e.g., below a temperature of 1080° C.), consolidated preform blocks that, prior to pressing, have interposed between the consolidated powder metal blocks at least one continuous solid interface portion. The at least one continuous solid interface portion may include a cold spray body, which may be a mass of cold spray deposited powders on a surface a block, a sintered preform, a compacted powder body (e.g., a tile), or any combination thereof.

Claims (56)

1. A method for making a sputtering target, comprising the steps of:

a. providing first and second at least partially consolidated powder metal blocks each having a prepared surface, and each including an alloy including molybdenum in an amount greater than about 30 percent by weight and at least one additional alloying element;

b. interposing between the consolidated powder metal blocks at least one continuous solid interface portion;

c. contacting the prepared surface of the first block indirectly with the prepared surface of the second block via the at least one continuous solid interface portion in the substantial absence of any loose powder bonding agent between contacted surfaces to form a contacted joint structure;

d. isostatically pressing the contacted structure at a temperature that is less than about 1080° C. at a pressure and for a time sufficient to realize a consolidated joint between the first and second blocks;

wherein the interposing step includes a step selected from

(i) cold spraying a metal powder onto at least one of the blocks for forming the at least one continuous solid interface portion;

(ii) compacting a body of metal powder to form the at least one continuous solid interface portion;

(iii) sintering a body of a metal powder mixture to form the at least one continuous solid interface portion;

(iv) cold spraying a metal powder into a die for forming the at least one continuous solid interface portion;

(v) cold spraying a metal powder onto a substrate to form the at least one continuous solid interface portion that may include or omit the substrate; or

(vi) any combination of (i) through (v).

2. The method of claim 1 , wherein the step of providing includes a step of forming the first and second blocks from an alloy that includes molybdenum, and at least one alloying element selected from titanium, chromium, niobium, tantalum, tungsten, zirconium or any combination thereof.

3. The method of claim 1 , wherein the step of isostatically pressing includes pressing at a temperature between about 500 and about 1080° C. while the contacted structure is encapsulated in a sealed vessel.

4. The method of claim 3 , wherein the step of isostatically pressing includes pressing at a pressure of at least about 70 MPa while the contacted structure is encapsulated in a sealed vessel.

5. The method of claim 1 , wherein the step of isostatically pressing includes maintaining a pressure of about 80 to about 140 MPa at a temperature of about 700° C. to about 1080° C. for a time of about one to about six hours while the contacted structure is encapsulated in a sealed vessel.

6. The method of claim 5 , wherein the at least one alloying element is titanium; and the step of isostatically pressing is performed under conditions sufficient so that a microstructure is realized that is characterized as including a pure titanium phase, a pure molybdenum phase and an alloy phase of titanium and molybdenum.

7. The method claim 6 , wherein the step of isostatically pressing is performed under conditions sufficient so that the resulting consolidated joint provides a structure that has a transverse rupture strength per ASTM B528-10, of at least about 620 MPa.

8. The method of claim 7 , wherein a resulting oxygen weight concentration of the blocks of the sputtering target is between about 1000 ppm and 3500 ppm.

9. The method of claim 1 , wherein the resulting sputtering target includes at least one continuous solid interface portion derived from a cold spray deposition, a sintered preform body, a compacted powder body or any combination thereof; and a joint between the at least partially consolidated blocks, which joins the blocks together to define a target body, the joint including the at least one continuous solid interface portion, wherein the sputtering target along the joint exhibits a transverse rupture strength per ASTM B528-10, of at least about 600 MPa.

10. The method of claim 1 , wherein the first and second at least partially consolidated powder metal blocks are formed from powder that is first compacted to about 60 to about 85% of theoretical density and then further densified prior to forming the joint; and the joint exhibits a transverse rupture strength per ASTM B528-10, of at least 600 MPa.

11. The method of claim 10 , wherein the resulting sputtering target includes a target body defined by the consolidated powder metal blocks and the joint formed from the continuous solid interface portion, wherein throughout the target body there is a substantially continuous and uniform distribution of three phases including a substantially pure molybdenum phase, a substantially pure phase of the at least one additional alloying element and a third phase that includes an alloy of molybdenum and the at least one additional alloying element.

12. The method of claim 11 , wherein the at least one additional alloying element includes titanium.

13. The method of claim 12 , wherein the amount of the substantially pure molybdenum phase is about 30 to about 60 vol % of the sputtering target body.

14. The method of claim 13 , wherein the amount of the substantially pure phase of the at least one additional alloying element is about 5 to about 25 vol %.

15. The method of claim 14 , wherein the alloy of molybdenum and the at least one additional alloying element includes a β-phase of molybdenum and titanium, in an amount greater than about 40 vol % of the alloy, of the target, or both.

16. The process of claim 1 , wherein the resulting sputtering target comprises:

a. the at least two consolidated blocks;

b. the at least one continuous solid interface portion; and

c. a joint between the at least two consolidated blocks, which joins the blocks together to define a target body, the joint including the at least one continuous solid interface portion,

wherein the resulting sputtering target along the joint exhibits a transverse rupture strength per ASTM B528-10, of at least about 400 MPa.

17. A method for making a sputtering target, comprising the steps of:

a) providing first and second at least partially consolidated powder metal blocks each optionally having a prepared surface, and each including an alloy including a refractory metal in an amount greater than 30 percent by weight and at least one additional alloying element;

b) interposing between the consolidated powder metal blocks at least one continuous solid interface portion, wherein the continuous solid interface portion is derived from a cold spray deposition onto a surface of at least one of the consolidated powder metal blocks, wherein the cold spray deposition has a porosity from 5 to 25% by volume as measured by ASTM B962-08 prior to the formation of the joint;

c) contacting the prepared surface of the first consolidated powder metal block indirectly with the prepared surface of the second consolidated powder metal block via the at least one continuous solid interface portion in the substantial absence of any bonding agent between the contacted surfaces to form a contacted joint structure; and

d) isostatically pressing the contacted structure at a temperature that is less than 1080° C. at a pressure and for a time sufficient to realize a consolidated joint between the first and second consolidated powder metal blocks.

18. The method of claim 17 , wherein

the first and second at least partially consolidated powder metal blocks are formed from powder that is first compacted to about 60 to about 85% of theoretical density and then further densified prior to forming the joint;

the resulting sputtering target includes a target body defined by the consolidated powder metal blocks and the joint formed from the continuous solid interface portion, wherein throughout the target body there is a substantially continuous and uniform distribution of three phases including a substantially pure molybdenum phase, a substantially pure phase of the at least one additional alloying element and a third phase that includes an alloy of molybdenum and the at least one additional alloying element; and

the at least one alloying element includes titanium, chromium, niobium, tantalum, tungsten, zirconium or any combination thereof.

19. The method of claim 18 , wherein

the at least one additional alloying element includes titanium;

the amount of the substantially pure molybdenum phase is about 30 to about 60 vol % of the sputtering target body;

the amount of the substantially pure phase of the at least one additional alloying element is about 5 to about 25 vol %; and

the alloy of molybdenum and the at least one additional alloying element includes a 8-phase of molybdenum and titanium, in an amount greater than about 40 vol % of the alloy, of the target, or both.

20. The method of claim 19 , wherein the joint exhibits a transverse rupture strength of at least 600 MPa as measured according to ASTM B528-10.

21. A method for making a sputtering target, comprising the steps of:

a. providing first and second at least partially consolidated powder metal blocks each having a prepared surface, and each including an alloy including molybdenum in an amount greater than about 30 percent by weight and at least one additional alloying element;

b. interposing between the consolidated powder metal blocks at least one continuous solid interface portion;

c. contacting the prepared surface of the first block indirectly with the prepared surface of the second block via the at least one continuous solid interface portion in the substantial absence of any loose powder bonding agent between contacted surfaces to form a contacted joint structure;

d. isostatically pressing the contacted structure at a temperature that is less than about 1080° C. at a pressure and for a time sufficient to realize a consolidated joint between the first and second blocks;

wherein the continuous solid interface portion is

i) a cold spray deposition having a porosity of 5 to 25% by volume as measured by ASTM B962-08 prior to the step of isostatically pressing the contacted structure; or

ii) a tile having a density of 60% to 85% of theoretical density prior to the step of isostatically pressing the contacted structure.

22. The method of claim 21 , wherein the continuous solid interface portion is a cold spray deposition having a porosity of 5 to 25% by volume as measured by ASTM B962-08 prior to the step of isostatically pressing the contacted structure.

23. The method of claim 21 , wherein the continuous solid interface portion is a tile having a density of 60% to 85% of theoretical density prior to the step of isostatically pressing the contacted structure.

Assignments (8)
SECURITY INTEREST Recorded Nov 6, 2023
From: H.C. STARCK SOLUTIONS COLDWATER, LLC; H.C. STARCK SOLUTIONS EUCLID, LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 065472/0843 →
CHANGE OF NAME Recorded Nov 1, 2023
From: EUCLID FACILITY HOLDINGS, LLC
To: H.C. STARCK SOLUTIONS EUCLID, LLC
Reel/Frame 065415/0762 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 31, 2023
From: H.C. STARCK INC.
To: EUCLID FACILITY HOLDINGS, LLC
Reel/Frame 065402/0594 →
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 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 Apr 26, 2013
From: ROZAK, GARY ALAN; GAYDOS, MARK E.; MICHALUK, CHRISTOPHER
To: H.C. STARCK, INC.
Reel/Frame 030294/0466 →