Method for producing inorganic oxide in form of thin film

Patent metadata

Field	Value
Publication number	US-11066302-B2
Application number	US-201716324441-A
Country	US
Kind code	B2
Filing date	Aug 8, 2017
Priority date	Aug 9, 2016
Publication date	Jul 20, 2021
Grant date	Jul 20, 2021

Abstract

Provided is a method for producing an inorganic oxide in the form of a thin film, the method including a step of bringing a first liquid and a second liquid into contact with each other, the first liquid having an inorganic oxide precursor dissolved therein, the second liquid phase-separating from the first liquid and having a substance dissolved therein, the substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide derived from the inorganic oxide precursor. The segment size of the first liquid at the time of contact between the first and second liquids is 500 μm or smaller.

First claim

The invention claimed is:

1. A method for producing an inorganic oxide in a form of a thin film, the method comprising
providing a stream of a first liquid having an inorganic oxide precursor dissolved therein,
providing a separate stream of a second liquid having a substance dissolved therein, the substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide derived from the inorganic oxide precursor, and
bringing said first liquid and said second liquid into contact with each other,
wherein a segment size of a cross-section perpendicular to a flow direction of the first liquid at a time of contact between the first and second liquids is maintained at 500 μm or smaller, thereby providing an inorganic oxide in the form of a thin film having an average thickness of 0.01 μm or larger and 1.5 μm or smaller.

2. The method of claim 1 , wherein
the bringing the first liquid and the second liquid into contact with each other is performed by continuous operation.

3. The method of claim 2 , wherein
a mode of contact between the first and second liquids includes a mode of supplying moving one of the first and second liquids with another to bring the first and second liquids into contact with each other.

4. The method of claim 3 , wherein
the mode of contact between the first and second liquids includes a mode of supplying transported one of the first and second liquids with another to bring the first and second liquids into contact with each other.

5. The method of claim 3 , wherein
the mode of contact between the first and second liquids includes a mode of supplying flowing one of the first and second liquids with another to bring the first and second liquids into contact with each other.

6. The method of claim 5 , wherein
the mode of contact between the first and second liquids includes a mode of allowing both of the first and second liquids to flow and join together.

7. The method of claim 6 , wherein
a manner of supplying one of the first and second liquids with another is a manner of allowing both of the first and second liquids to flow out of slits and join together.

8. The method of claim 6 , wherein
the mode of contact between the first and second liquids includes a mode of allowing both of the first and second liquids to flow in a same flow direction, and, while maintaining the flow direction, bringing the first and second liquids into contact with each other.

9. The method of claim 8 , wherein
the manner of supplying one of the first and second liquids with another is a manner of allowing the one to flow between an inner pipe and an outer pipe of a double pipe while allowing the other to flow through the inner pipe, and causing the one and the other to join together so as to cover the other with the one.

10. The method of claim 6 , wherein
when both of the first and second liquids are allowed to flow, a ratio of a linear flow velocity of the first liquid to a linear flow velocity of the second liquid at a time of contact between the first liquid and the second liquid is 0.01 or more and 100 or less.

11. The method of claim 1 , wherein
the inorganic oxide precursor includes a metal alkoxide.

12. The method of claim 1 , wherein when the second liquid is allowed to flow, a Reynolds number of the second liquid until a time when the first and second liquids come into contact with each other is 0.01 or more and 500 or less.

13. The method of claim 1 , wherein
a segment size of the second liquid at the time of contact between the first liquid and the second liquid is 5 mm or smaller.

14. The method of claim 1 , wherein
a ratio of the segment size of the second liquid to the segment size of the first liquid at the time of contact between the first and second liquids is 0.1 or more and 500 or less.

15. The method of claim 1 , wherein
a solvent of the first liquid includes one or two or more of toluene, hexane, heptane, benzene, and chloroform.

16. The method of claim 1 , wherein
an interfacial tension of the first liquid to the second liquid at a temperature at the time of contact between the first liquid and the second liquid is 0.1 mN/m or more and 30 mN/m or less.

17. The method of claim 1 , wherein
a duration of contact between the first and second liquids is 0.5 sec or longer and 600 sec or shorter.

18. The method of claim 1 , wherein
a reaction temperature at the time of contact between the first and second liquids is 10° C. or higher and 60° C. or lower.

19. The method of claim 1 , wherein
a ratio of an average longitudinal diameter to the average thickness of the inorganic oxide in the form of the film is 5 or more and 2000 or less.

20. The method of claim 1 , wherein
a content of the inorganic oxide precursor in the first liquid is 1% by mass or more to 80% by mass or less.

21. The method of claim 1 , wherein
a content of the substance in the second liquid to form the inorganic oxide is 0.1% by mass or more to 70% by mass or less.

22. The method of claim 1 , wherein
a solvent of the second liquid includes at least one of ionic liquids, acetonitrile, and dimethyl sulfoxide.

23. A method for producing an inorganic oxide in a form of a thin film, the method comprising
providing a stream of a first liquid having an inorganic oxide precursor dissolved therein, providing a separate stream of a second liquid having a substance dissolved therein, the substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide derived from the inorganic oxide precursor, and
bringing said first liquid and said second liquid into contact with each other,
wherein a segment size of a cross-section perpendicular to a flow direction of the first liquid at a time of contact between the first and second liquids is maintained at 500 μm or smaller, thereby providing an inorganic oxide in the form of a thin film, and
wherein a ratio of an average longitudinal diameter to the average thickness of the inorganic oxide in the form of the film is 5 or more and 2000 or less.

Assignees

• Kao Corp

Inventors

• Onishi Ryo
• Oda Tsuyoshi

Classifications

• B05D3/00

  Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials (successively applying liquids or other fluent materials B05D1/36; drying ovens F26B) · CPC title

• C01G23/04

  Oxides; Hydroxides · CPC title

• C01B13/326 Primary

  of elements or compounds in the liquid state · CPC title

• C04B2235/441

  Alkoxides, e.g. methoxide, tert-butoxide · CPC title

• C01B13/32

  by oxidation or hydrolysis of elements or compounds in the liquid or solid state {or in non-aqueous solution, e.g. sol-gel process} · CPC title