IP Library Granted Patent US 10,526,697
Granted Patent B2
US 10,526,697 · App. 15/556,102 · Granted Jan 7, 2020

High-purity tungsten hexacarbonyl for solid source delivery

Inventors: Thomas H. Baum (New Fairfield, CT); Robert L. Wright, Jr. (Newtown, CT); Scott L. Battle (Cedar Park, TX); John M. Cleary (New Fairfield, CT)
Assignee: ENTEGRIS, INC.
C23C16/16C01G41/006
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 10,526,697
App. No.
15/556,102
Granted
Jan 7, 2020
Kind
B2
Abstract

A solid source material is described for forming a tungsten-containing film. The solid source material is tungsten hexacarbonyl, wherein content of molybdenum is less than 1000 ppm. Such solid source material may be formed by a process including provision of particulate tungsten hexacarbonyl raw material of particles of size less than 5 mm, wherein particles of size greater than 1.4 mm are less than 15% of the particles, and wherein content of molybdenum is less than 1000 ppm, and sintering the particulate tungsten hexacarbonyl raw material at temperature below 100° C. to produce the solid source material as a sintered solid.

Claims (20)

1. A solid source material for forming a tungsten-containing film by vapor deposition, which is a sintered tungsten hexacarbonyl consolidated from particulate tungsten hexacarbonyl at a temperature below 100° C., wherein the solid source material has a content of molybdenum that is less than 1000 ppm.

2. The solid source material of claim 1 , wherein the content of molybdenum is less than 300 ppm.

3. The solid source material of claim 1 , wherein the content of molybdenum is less than 10 ppm.

4. The solid source material of claim 1 , wherein the particulate tungsten hexacarbonyl is a particulate of particles of size less than 5 mm.

5. The solid source material of claim 4 , wherein particles of size greater than 1.4 mm are less than 15% of the particles.

6. The solid source material of claim 4 , wherein particles of size 0.25 mm to 1.4 mm are at least 50% of the particles.

7. The solid source material of claim 4 , wherein particles of size 0.25 mm to 1.4 mm are at least 70% of the particles.

8. The solid source material of claim 4 , wherein at least 80% of the particles are particles of size below 0.25 mm.

9. A process for forming a solid source material for forming a tungsten-containing film by vapor deposition, comprising:

providing particulate tungsten hexacarbonyl raw material of particles of size less than 5 mm, wherein particles of size greater than 1.4 mm are less than 15% of the particles, and wherein content of molybdenum is less than 1000 ppm; and

sintering the particulate tungsten hexacarbonyl raw material at temperature below 100° C. to produce the solid source material for forming a tungsten-containing film by vapor deposition, as a sintered solid.

10. The process of claim 9 , wherein the sintering comprises cold sintering.

11. The process of claim 9 , wherein content of molybdenum in the particulate tungsten hexacarbonyl raw material is less than 300 ppm.

12. The process of claim 9 , wherein content of molybdenum in the particulate tungsten hexacarbonyl raw material is less than 10 ppm.

13. The process of claim 9 , wherein particles of size 0.25 mm to 1.4 mm are at least 50% of the particles.

14. The process of claim 9 , wherein particles of size 0.25 mm to 1.4 mm are at least 70% of the particles.

15. A method of forming a tungsten-containing film on a substrate, comprising volatilizing a solid source material as claimed in claim 1 , to form a tungsten solid source material vapor, and contacting the tungsten solid source material vapor with a substrate under vapor deposition conditions, to form the tungsten-containing film on the substrate.

16. The method of claim 15 , wherein the contacting is carried out at temperature below 200° C.

17. The method of claim 15 , wherein the contacting is carried out at temperature below 100° C.

18. A tungsten solid source material supply package, comprising a vessel containing a solid source material as claimed in claim 1 .

Assignments (4)
SECURITY INTEREST Recorded Jul 8, 2022
From: ENTEGRIS, INC.; ENTEGRIS GP, INC.; POCO GRAPHITE, INC.; CMC MATERIALS, INC.; INTERNATIONAL TEST SOLUTIONS, LLC; QED TECHNOLOGIES INTERNATIONAL, INC.
To: TRUIST BANK, AS NOTES COLLATERAL AGENT
Reel/Frame 060613/0072 →
ASSIGNMENT OF PATENT SECURITY INTEREST RECORDED AT REEL/FRAME 048811/0679 Recorded Nov 5, 2019
From: GOLDMAN SACHS BANK USA
To: MORGAN STANLEY SENIOR FUNDING, INC.
Reel/Frame 050965/0035 →
SECURITY INTEREST Recorded Nov 13, 2018
From: ENTEGRIS, INC.; SAES PURE GAS, INC.
To: GOLDMAN SACHS BANK USA
Reel/Frame 048811/0679 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 19, 2018
From: BAUM, THOMAS H.; WRIGHT, ROBERT L.; CLEARY, JOHN M.; BATTLE, SCOTT L.
To: ENTEGRIS, INC.
Reel/Frame 047232/0317 →
Continuity (2)
Provisional Application 62129368 · Mar 6, 2015
Related Publication 20180044787A1 · Feb 15, 2018
Cited By (2)
US 12,319,999 US 12,577,663