Sol-gel process for synthesis of nanocrystalline oxides
US-10106432-B2 · Oct 23, 2018 · US
US11084733B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11084733-B2 |
| Application number | US-201716324466-A |
| Country | US |
| Kind code | B2 |
| Filing date | Aug 8, 2017 |
| Priority date | Aug 9, 2016 |
| Publication date | Aug 10, 2021 |
| Grant date | Aug 10, 2021 |
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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 with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide derived from the inorganic oxide precursor. The step is performed by continuous operation. At least one of the first liquid and the second liquid includes an ionic liquid.
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The invention claimed is: 1. A method for producing an inorganic oxide in a form of a thin film, the method comprising bringing a first liquid and a second liquid into contact with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide, derived from the inorganic oxide precursor, in the form of a thin film, wherein the inorganic oxide in the form of the thin film has a ratio of an average longitudinal diameter to an average thickness is 5 or more and 2000 or less, and the bringing of the first liquid into contact with the second liquid is performed by continuous operation, and at least one of the first liquid and the second liquid includes an ionic liquid. 2. The method of claim 1 , wherein the inorganic oxide in the form of the thin film has an average thickness of 0.01 μm or larger and 1.5 μm or smaller. 3. The method of claim 1 , wherein the inorganic oxide in the form of the thin film includes a titanium oxide in a form of a thin film. 4. The method of claim 1 , wherein the first liquid and the second liquid phase-separate from each other. 5. The method of claim 1 , wherein the ionic liquid includes an ionic liquid having 1-alkyl-3-methylimidazolium cations. 6. The method of claim 1 , wherein the inorganic oxide precursor includes a metal alkoxide. 7. The method of claim 1 , wherein the second liquid is a solution in which the substance to form the inorganic oxide is dissolved in the ionic liquid. 8. The method of claim 1 , wherein the first liquid is a solution in which the inorganic oxide precursor is dissolved in an organic solvent. 9. The method of claim 1 , wherein the first liquid contains one or two or more of toluene, hexane, heptane, benzene, and chloroform. 10. The method of claim 1 , wherein an interfacial tension of the first liquid to the second liquid at a temperature of 25° C. at a time of contact between the first liquid and the second liquid is 0.1 mN/m or more and 30 mN/m or less. 11. The method of claim 1 , wherein when both of the first liquid and the second liquid flow to contact one another, 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. 12. The method of claim 1 , wherein when both of the first liquid and the second liquid flow to contact one another, a ratio of a Reynolds number of the first liquid to a Reynolds number of the second liquid until a time when the first liquid and the second liquid come into contact with each other is 4 or more and 1000 or less. 13. The method of claim 1 , wherein a duration of contact between the first liquid and the second liquid is 0.5 sec or longer and 600 sec or shorter. 14. The method of claim 1 , wherein a reaction temperature at a time of contact between the first liquid and the second liquid is 0° C. or higher and 100° C. or lower. 15. The method of claim 1 , wherein the inorganic oxide in the form of the thin film has an average longitudinal diameter of 2 μm or larger and 300 μm or smaller. 16. The method of claim 1 , wherein the ionic liquid includes ammonium cations. 17. The method of claim 1 , wherein the ionic liquid includes 1-methyl-3-methylimidazolium cations, 1-ethyl-3-methylimidazolium cations, 1-propyl-3-methylimidazolium cations, or 1-butyl-3-methylimidazolium cations. 18. The method of claim 1 , wherein the inorganic oxide precursor includes a titanium alkoxide or a zirconium alkoxide. 19. The method of claim 18 , wherein the titanium alkoxide includes tetraethyl orthotitanate, tetraisopropyl orthotitanate, or tetra-n-butyl orthotitanate. 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. A method for producing an inorganic oxide in a form of a thin film, the method comprising bringing a first liquid and a second liquid into contact with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide, derived from the inorganic oxide precursor, in the form of a thin film, the bringing of the first liquid into contact with the second liquid is performed by continuous operation, and at least one of the first liquid and the second liquid includes an ionic liquid, and wherein an interfacial tension of the first liquid to the second liquid at a temperature of 25° C. at a time of contact between the first liquid and the second liquid is 0.1 mN/m or more and 30 mN/m or less. 23. A method for producing an inorganic oxide in a form of a thin film, the method comprising bringing a first liquid and a second liquid into contact with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide, derived from the inorganic oxide precursor, in the form of a thin film, the bringing of the first liquid into contact with the second liquid is performed by continuous operation, and at least one of the first liquid and the second liquid includes an ionic liquid, and wherein when both of the first liquid and the second liquid flow to contact one another, 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. 24. A method for producing an inorganic oxide in a form of a thin film, the method comprising bringing a first liquid and a second liquid into contact with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide, derived from the inorganic oxide precursor, in the form of a thin film, the bringing of the first liquid into contact with the second liquid is performed by continuous operation, and at least one of the first liquid and the second liquid includes an ionic liquid, and wherein when both of the first liquid and the second liquid flow to contact one another, a ratio of a Reynolds number of the first liquid to a Reynolds number of the second liquid until a time when the first liquid and the second liquid come into contact with each other is 4 or more and 1000 or less. 25. A method for producing an inorganic oxide in a form of a thin film, the method comprising bringing a first liquid and a second liquid into contact with each other, the first liquid containing an inorganic oxide precursor and the second liquid containing a substance reacting with the inorganic oxide precursor of the first liquid to form an inorganic oxide, derived from the inorganic oxide precursor, in the form of a thin film, the bringing of the first liquid into contact with the second liquid is performed by continuous operation, and at least one of the first liquid and the second liquid includes an ionic liquid, and wherein the inorganic oxide in the form
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