Method of producing composite photocatalyst

Patent metadata

Field	Value
Publication number	US-11424080-B2
Application number	US-201916400461-A
Country	US
Kind code	B2
Filing date	May 1, 2019
Priority date	Nov 21, 2014
Publication date	Aug 23, 2022
Grant date	Aug 23, 2022

Abstract

The present invention provides a method of producing a composite photocatalyst having a remarkable water splitting activity, which is capable of efficiently loading a co-catalyst having a small particle size in a highly dispersed manner on a surface of an optical semiconductor. According to the present invention, the method of producing a composite photocatalyst from a plurality types of optical semiconductors includes a step of heating a solid-liquid mixture containing a solvent, a co-catalyst or a co-catalyst source, and a plurality of types of optical semiconductors by irradiating the solid-liquid mixture with microwave.

First claim

The invention claimed is:

1. A method of producing a composite photocatalyst from a plurality of types of optical semiconductors, the method comprising:
heating a solid-liquid mixture comprising a solvent, a co-catalyst or a co-catalyst source, and the plurality of types of optical semiconductors, by irradiating the solid-liquid mixture with microwave irradiation, thereby bonding the plurality of types of the optical semiconductors to each other with the co-catalyst interposed therebetween and/or with the co-catalyst covering the optical semiconductors.

2. The method of claim 1 , wherein before the microwave irradiation, the co-catalyst source is present in the solid-liquid mixture and is dissolved in a solvent.

3. The method of claim 1 , wherein the co-catalyst is loaded on the surface of the optical semiconductors has coverage per unit area of the optical semiconductors due to the co-catalyst is equal to or greater than 30%.

4. The method of claim 1 , wherein the co-catalyst has a particle size of equal to or smaller than 20 nm.

5. The method of claim 1 , wherein the co-catalyst has a particle size of equal to or smaller than 15 nm.

6. The method of claim 1 , wherein the co-catalyst has a particle size of equal to or smaller than 10 nm.

7. The method of claim 1 , wherein, before the microwave irradiation, the co-catalyst and the optical semiconductor are present in the solid-liquid mixture as a solid in the solvent, and the co-catalyst is loaded on the optical semiconductor.

8. The method of claim 7 , further comprising, before the heating:
first loading a co-catalyst on a first optical semiconductor by microwave heating in a state where the first optical semiconductor is brought into contact with a solution in which a co-catalyst source is dissolved, to obtain a loaded first optical semiconductor;
second loading a co-catalyst on a second optical semiconductor by microwave heating in a state where the second optical semiconductor is brought into contact with the solution in which the co-catalyst source is dissolved, to obtain a loaded second optical semiconductor; and
mixing the loaded first optical semiconductor and the loaded second optical semiconductor, into the solvent so as to obtain the solid-liquid mixture.

9. The method of claim 8 , wherein the microwave irradiation is performed in a closed system in the first loading and the second loading.

10. The method of claim 8 , further comprising before the first loading and the second loading:
bringing a solution comprising an organic acid comprising a polyorganic acid into contact with a surface of an oxide, an oxynitride, or a nitride comprising Ti, V, Ga, Ge, Nb, La, and/or Ta; and
collecting the oxide, the oxynitride, or the nitride remaining as a solid content after the contacting with the organic acid(s),
wherein the collected solid contents are used as the first optical semiconductor and the second optical semiconductor.

11. The method of claim 1 , wherein the plurality of types of optical semiconductors comprises an oxide, a nitride, an oxynitride, a chalcogenide, or an oxychalcogenide, comprising Ti, V, Ga, In, Bi, Nb, and/or Ta.

12. The method of claim 11 , wherein the plurality of types of optical semiconductors comprises BaTaO 2 N, BaNbO 2 N, TaON, Ta 3 N 5 , LaTiO 2 N, BiVO 4 , and/or GaN:ZnO, or a partial substitution thereof.

13. The method of claim 1 , wherein the co-catalyst or the co-catalyst source comprises Co or Co-ion.

14. The method of claim 1 , wherein the solvent comprises water, an alcohol, or a mixture of two or more of these.

15. The method of claim 1 , wherein the heating comprises irradiating the solid-liquid mixture with the microwave in a closed system.

16. The method of claim 15 , wherein pressure in the closed system is higher than pressure outside the system.

17. The method of claim claim 1 , further comprising, before the heating:
bringing a solution comprising an organic acid comprising a polyorganic acid into contact with a surface of an oxide, an oxynitride, or a nitride, comprising Ti, V, Ga, Ge, Nb, La, and/or Ta; and
collecting the oxide, the oxynitride, or the nitride remaining as a solid content after the contacting with the organic acid(s),
wherein the collected solid contents are used as the optical semiconductor.

18. The method of claim 17 , wherein the organic acid is a polysulfonic acid.

19. The method of claim 17 , wherein the organic acid comprises an aryl group.

20. The method of claim 17 , wherein the organic acid has a weight average molecular weight in a range of from 1,000 to 1,000,000.

Assignees

• Mitsubishi Chem Corp
• Univ Tokyo
• Japan Tech Research Association Of Artificial Photosynthetic Chemical Process

Inventors

• Akiyama Seiji
• Domen Kazunari

Classifications

• C25B1/04

  by electrolysis of water · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• Y02E60/36

  Hydrogen production from non-carbon containing sources, e.g. by water electrolysis · CPC title

• B01J27/24 Primary

  Nitrogen compounds · CPC title