Tungsten hexafluoride manufacturing method, tungsten hexafluoride purification method, and tungsten hexafluoride

Patent metadata

Field	Value
Publication number	US-12304833-B2
Application number	US-202017442446-A
Country	US
Kind code	B2
Filing date	Mar 19, 2020
Priority date	Mar 25, 2019
Publication date	May 20, 2025
Grant date	May 20, 2025

Abstract

A tungsten hexafluoride manufacturing method of the present invention includes a reaction step of reacting tungsten containing arsenic or an arsenic compound with a gas of a fluorine element-containing compound so as to obtain a mixture containing tungsten hexafluoride and a trivalent arsenic compound, and a distillation step of distilling and purifying the mixture so as to separate and remove a fraction containing the trivalent arsenic compound and to obtain tungsten hexafluoride.

First claim

The invention claimed is:

1. A method of manufacturing tungsten hexafluoride, comprising:
a reaction step comprising reacting tungsten containing arsenic or an arsenic compound with a gas of a fluorine element-containing compound, so as to obtain a mixture comprising tungsten hexafluoride and a trivalent arsenic compound; and
a distillation step comprising distilling and purifying the mixture so as to separate and remove a first fraction comprising the trivalent arsenic compound and to obtain tungsten hexafluoride.

2. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein the reaction step further comprises reacting the tungsten containing arsenic or an arsenic compound with the gas of a fluorine element-containing compound, so as to obtain an intermediate product containing a pentavalent arsenic compound and tungsten hexafluoride, and a step of bringing the intermediate product into contact with a reducing substance so as to convert at least a part of the pentavalent arsenic compound into a trivalent arsenic compound and to obtain the mixture.

3. The method of manufacturing tungsten hexafluoride according to claim 2 ,
wherein the reducing substance comprises at least one substance selected from the group consisting of tungsten, molybdenum, copper, nickel, iron, cobalt, zinc, titanium, aluminum, calcium, magnesium, phosphorus, and hydrogen.

4. The method of manufacturing tungsten hexafluoride according to claim 2 ,
wherein the intermediate product and the reducing substance are brought into contact with each other under a temperature condition of 100° C. to 500° C.

5. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein an amount of the first fraction separated and removed is 0.1% by mass to 5% by mass with respect to a feed amount of 100% by mass of the tungsten hexafluoride subjected to the distillation step.

6. The method of manufacturing tungsten hexafluoride according to claim 1 , further comprising, after the distillation step:
a filling step of vaporizing the tungsten hexafluoride and filling a storage container with the tungsten hexafluoride.

7. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein the trivalent arsenic compound comprises arsenic trifluoride.

8. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein in the distillation step, the first fraction is separated and removed to obtain tungsten hexafluoride satisfying the following condition:
a content of the trivalent arsenic compound in the tungsten hexafluoride obtained after the distillation step is equal to or less than 100 ppb by mass in terms of arsenic atoms.

9. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein the distillation step is performed with a distillation apparatus comprising a distillation column.

10. The method of manufacturing tungsten hexafluoride according to claim 9 ,
wherein the tungsten hexafluoride is refluxed in the distillation column.

11. The method of manufacturing tungsten hexafluoride according to claim 1 ,
wherein the tungsten hexafluoride obtained after the distillation step is used as a raw material gas for chemical vapor deposition (CVD).

12. A method of manufacturing tungsten hexafluoride, comprising:
a reaction step comprising reacting tungsten containing arsenic or an arsenic compound with a gas of a fluorine element-containing compound, so as to obtain an intermediate product comprising a pentavalent arsenic compound and tungsten hexafluoride, and a step of bringing the intermediate product into contact with a reducing substance so as to convert at least a part of the pentavalent arsenic compound into a trivalent arsenic compound and to obtain a mixture; and
a distillation step comprising distilling and purifying the mixture so as to separate and remove a fraction comprising the trivalent arsenic compound and to obtain tungsten hexafluoride.

13. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein the reducing substance comprises at least one substance selected from the group consisting of tungsten, molybdenum, copper, nickel, iron, cobalt, zinc, titanium, aluminum, calcium, magnesium, phosphorus, and hydrogen.

14. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein the intermediate product and the reducing substance are brought into contact with each other under a temperature condition of 100° C. to 500° C.

15. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein an amount of the first fraction separated and removed is 0.1% by mass to 5% by mass with respect to a feed amount of 100% by mass of the tungsten hexafluoride subjected to the distillation step.

16. The method of manufacturing tungsten hexafluoride according to claim 12 , further comprising, after the distillation step:
a filling step of vaporizing the tungsten hexafluoride and filling a storage container with the tungsten hexafluoride.

17. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein the trivalent arsenic compound comprises arsenic trifluoride.

18. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein in the distillation step, the first fraction is separated and removed to obtain tungsten hexafluoride satisfying the following condition:
a content of the trivalent arsenic compound in the tungsten hexafluoride obtained after the distillation step is equal to or less than 100 ppb by mass in terms of arsenic atoms.

19. The method of manufacturing tungsten hexafluoride according to claim 12 ,
wherein the distillation step is performed with a distillation apparatus comprising a distillation column.

20. The method of manufacturing tungsten hexafluoride according to claim 19 ,
wherein the tungsten hexafluoride is refluxed in the distillation column.

Assignees

• Central Glass Co Ltd

Inventors

• Ohashi Mitsuya
• Hamana Takanori
• Ogata Takanori
• Nakamura Ryuichi

Classifications

• B01D3/14

  Fractional distillation {or use of a fractionation or rectification column} · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C01G41/04 Primary

  Halides · CPC title