Tungsten pentachloride conditioning and crystalline phase manipulation

Patent metadata

Field	Value
Publication number	US-10899630-B2
Application number	US-201816144000-A
Country	US
Kind code	B2
Filing date	Sep 27, 2018
Priority date	Apr 30, 2018
Publication date	Jan 26, 2021
Grant date	Jan 26, 2021

Abstract

A process of conditioning tungsten pentachloride to form specific crystalline phases are disclosed. The specific crystalline phases permit stable vapor pressures over extended periods of time during vapor deposition and etching processes.

First claim

We claim:

1. A method of conditioning WCl 5 , the method comprising heating a container of WCl 5 to a temperature ranging from approximately 190° C. to 245° C. for a time period ranging from approximately 2 hours to approximately 48 hours to produce a WCl 5 -containing composition comprising a crystalline phase having approximately 10% weight to approximately 40% weight of Phase 1 WCl 5 as determined by X-ray diffraction.

2. The method of claim 1 , wherein the container is selected to be non-reactive to WCl 5 .

3. The method of claim 2 , wherein the container is glass or glass-lined.

4. The method of claim 3 , wherein the container is sealed.

5. The method of claim 1 , wherein the time period ranges from approximately 24 hours to approximately 48 hours.

6. The method of claim 5 , wherein the time period ranges from approximately 40 hours to approximately 48 hours.

7. The method of claim 1 , wherein the temperature ranges from approximately 215° C. to 240° C.

8. The method of claim 7 , wherein the temperature ranges from approximately 225° C. to 235° C.

9. The method of claim 1 , wherein the crystalline phase of the WCl 5 -containing composition comprises approximately 10% weight to approximately 35% weight of Phase 1 WCl 5 .

10. The method of claim 1 , wherein the crystalline phase of the WCl 5 -containing composition comprises approximately 10% weight to approximately 30% weight of Phase 1 WCl 5 .

11. A method of providing a vapor of WCl 5 having a vapor pressure, the method comprising heating a container comprising a WCl 5 -containing composition, the WCl 5 of the WCl 5 -containing composition having a crystalline phase having approximately 10% by weight to approximately 40% by weight of Phase 1 WCl 5 as determined by X-ray diffraction.

12. The method of claim 11 , wherein the container is a solid precursor vaporizer.

13. The method of claim 12 , further comprising connecting the solid precursor vaporizer to a semiconductor processing chamber and heating the solid precursor vaporizer to a delivery temperature to provide an initial vapor pressure of WCl 5 .

14. The method of claim 13 , wherein the WCl 5 -containing composition maintains approximately 80% w/w of the initial vapor pressure of WCl 5 at the delivery temperature after approximately 75% w/w of the WCl 5 -containing composition has been consumed.

Assignees

• Air Liquide

Inventors

• Li Feng
• Plaza Sonia
• Girard Jean-Marc
• Blasco Nicolas
• Liu Yumin

Classifications

• C01G41/04 Primary

  Halides · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title