Cryogenic annealing of sputtering targets

• US 6,056,857 A
• Filed: 08/13/1997
• Issued: 05/02/2000
• Est. Priority Date: 08/13/1997
• Status: Expired due to Term

• Current Assignee: Praxair S.T. Technology, Inc. (Linde Plc)
• Original Assignee: Praxair S.T. Technology, Inc. (Linde Plc)
• Inventors: Joyce, James E., Gilman, Paul S., Hunt, Thomas J., Lo, Chi-Fung, Draper, Darryl
• Primary Examiner(s): MCDONALD, RODNEY GLENN
• Application Number:
  US08/910,334
• Time in Patent Office: 993 Days
• Field of Search: 148/577, 204/192.1, 204/192.12, 204/192.15, 204/298.12, 204/298.13
• US Class Current: 204/192.15
• CPC Class Codes: C23C 14/3414 Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
• CPC Class Codes: C23C 14/564 Means for minimising impurities in the coating chamber such as dust, moisture, residual gases

Abstract

Sputtering targets are cryogenically annealed to provide a uniformly dense molecular structure by placing the target in a temperature-controlled cryogenic chamber and cooling the chamber to a cryogenic temperature at a controlled rate. The target is maintained at a cryogenic temperature to cryogenically anneal the target and the target is subsequently returned to ambient or elevated temperature. Improvements in sputtered particle performance and early life film uniformity are achieved with the cryo-annealed targets.

Claims

1. A method for cryogenically annealing a sputtering target to provide a uniformly dense molecular target structure comprising

placing a sputtering target having internal and external stresses in a temperature-controlled cryogenic chamber,

cooling said chamber with a liquified gas from an ambient temperature to a cryogenic temperature at a controlled rate to cool the target and avoid target fracture,

maintaining the target at said cryogenic temperature for a period of time sufficient to cryogenically anneal the target, whereby said internal and external stresses are relieved and a uniformly dense molecular target structure is provided, and

returning the target structure to ambient or elevated temperature.

2. The method of claim 1 wherein said target is returned to ambient temperature.

3. The method of claim 1 wherein said liquified gas is selected from the group including helium, hydrogen, argon, oxygen and nitrogen.

4. The method of claim 1 wherein said liquified gas is nitrogen.

5. The method of claim 1 wherein said cryogenic temperature is below about -175°

C.

6. The method of claim 4 wherein said chamber is cooled to about -185°

C. with liquid nitrogen.

7. The method of claim 1 wherein said chamber is cooled at the controlled rate of approximately 0.55°

C. per minute.

8. The method of claim 1 wherein said target is returned to ambient or elevated temperature at a controlled rate before removal from said chamber.

9. The method of claim 8 wherein said controlled rate returning said target to ambient or elevated temperature is approximately 0.55°

C. per minute.

10. The method of claim 1 wherein said target comprises a metal selected from the group consisting of aluminum, titanium, zirconium, hafnium, chromium, cobalt, nickel, tantalum, and tungsten, and mixtures thereof.

11. The method of claim 1 further comprising sputtering said target structure to deposit a film onto a substrate.

12. The method of claim 1 wherein said sputtering target is manufactured by pressing, forging, rolling and forming.

13. The method of claim 1 wherein the cooling, maintaining and returning steps are computer controlled.

14. A method for cryogenically annealing a sputtering target to provide a uniformly dense molecular target structure for improved sputtered particle performance and uniformity comprising

placing a sputtering target having internal and external stresses in a temperature-controlled cryogenic chamber,

cooling said chamber from an ambient temperature with liquid nitrogen to a cryogenic temperature of approximately -185°

C. at a computer-controlled rate to cool the target and to avoid target fracture,

maintaining the target at approximately -185°

C. for a period of time sufficient to cryogenically anneal the target, whereby said internal and external stresses are relieved and a uniformly dense molecular target structure is provided.

returning said target structure at a computer-controlled rate to an elevated temperature, and

removing said target from said chamber.

15. The method of claim 14 wherein said computer-controlled rate in the range of about -2°

C./min, to +2°

C./min.

16. The method of claim 14 wherein said sputtering target comprising a molded element of a metal selected from a group consisting of aluminum, titanium, zirconium, hafnium, chromium, cobalt, nickel, tantalum and tungsten, and mixtures thereof.