Molybdenum pentachloride conditioning and crystalline phase manipulation

Patent metadata

Field	Value
Publication number	US-12559859-B2
Application number	US-202318134494-A
Country	US
Kind code	B2
Filing date	Apr 13, 2023
Priority date	Apr 13, 2023
Publication date	Feb 24, 2026
Grant date	Feb 24, 2026

Abstract

A method of conditioning MoCl 5 comprises heating a container of MoCl 5 to a temperature ranging from approximately 140° C. to 190° C. for a period ranging from approximately 2 hours to approximately 100 hours to produce a MoCl 5 -containing composition comprising approximately 10% weight to approximately 60% weight of Phase 1 MoCl 5 and 90% weight to approximately 40% weight of Phase 2 MoCl 5 as determined by X-ray diffraction. This MoCl 5 -containing composition is expected to be more thermally stable and provides stable vapor supply.

First claim

What is claimed is:

1 . A method of conditioning MoCl 5 , the method comprising
heating a container of a mixture of Phase 1 and Phase 3 MoCl 5 that contains approximately 10% weight to approximately 90% weight of Phase 3 MoCl 5 to a temperature ranging from approximately 140° C. to 190° C. for a period ranging from approximately 2 hours to approximately 100 hours to produce a MoCl 5 -containing composition comprising approximately 10% weight to approximately 60% weight of Phase 1 MoCl 5 and 90% weight to approximately 40% weight of Phase 2 MoCl 5 , as determined by X-ray diffraction, wherein the Phase 3 MoCl 5 is transferred to the Phase 1 and Phase 2 MoCl 5 .

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

3 . The method of claim 1 , wherein the container is glass or glass-lined.

4 . The method of claim 1 , wherein the container is stainless steel.

5 . The method of claim 1 , wherein the container is glass, Teflon, or coated stainless steel.

6 . The method of claim 1 , wherein the period ranges from approximately 24 hours to approximately 72 hours.

7 . The method of claim 1 , wherein the period ranges from approximately 36 hours to approximately 48 hours.

8 . The method of claim 1 , wherein the temperature ranges from approximately 150° C. to 180° C.

9 . The method of claim 1 , wherein the temperature ranges from approximately 160° C. to 170° C.

10 . The method of claim 1 , wherein the MoCl 5 -containing composition comprises approximately 10% weight to approximately 60% weight of Phase 1 MoCl 5 and 90% weight to approximately 40% weight of Phase 2 MoCl 5 .

11 . The method of claim 1 , wherein the MoCl 5 -containing composition comprises approximately 20% weight to approximately 50% weight of Phase 1 MoCl 5 and 80% weight to approximately 50% weight of Phase 2 MoCl 5 .

12 . The method of claim 1 , wherein the MoCl 5 -containing composition comprises approximately 30% weight to approximately 55% weight of Phase 1 MoCl 5 and 70% weight to approximately 45% weight of Phase 2 MoCl 5 .

13 . The method of claim 1 , wherein the MoCl 5 -containing composition comprises approximately 40% weight to approximately 50% weight of Phase 1 MoCl 5 and 60% weight to approximately 50% weight of Phase 2 MoCl 5 .

14 . A MoCl 5 -containing composition conditioned by the method of claim 1 , having approximately 10% weight to approximately 60% weight of Phase 1 MoCl 5 and 90% weight to approximately 40% weight of Phase 2 MoCl 5 .

15 . The MoCl 5 -containing composition of claim 14 , having approximately 20% weight to approximately 50% weight of Phase 1 MoCl 5 and 80% weight to approximately 50% weight of Phase 2 MoCl 5 .

16 . The MoCl 5 -containing composition of claim 14 , having approximately 30% weight to approximately 55% weight of Phase 1 MoCl 5 and 70% weight to approximately 45% weight of Phase 2 MoCl 5 .

17 . The MoCl 5 -containing composition of claim 14 , having approximately 40% weight to approximately 50% weight of Phase 1 MoCl 5 and 60% weight to approximately 50% weight of Phase 2 MoCl 5 .

18 . The MoCl 5 -containing composition of claim 14 , being thermally stable and providing stable vapor supply.

Assignees

• Air Liquide
• Lair Liquide Sa Pour Letude Et Lexploitation Des Proceedes Georges Claude

Inventors

• Li Feng
• Liu Yumin
• Helmy Sameh
• Zhang Peng
• Girard Jean-Marc

Classifications

• C30B29/12 Primary

  Halides · CPC title

• C30B35/007

  Apparatus for preparing, pre-treating the source material to be used for crystal growth · CPC title

• C30B23/002 Primary

  Controlling or regulating · CPC title

• C23C16/52

  Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)} · CPC title

• C23C16/452

  by activating reactive gas streams before {their} introduction into the reaction chamber, e.g. by {ionisation} or addition of reactive species · CPC title