Macroporous titanium compound monolith and method for producing same

Patent metadata

Field	Value
Publication number	US-9902623-B2
Application number	US-201314379218-A
Country	US
Kind code	B2
Filing date	Feb 18, 2013
Priority date	Feb 17, 2012
Publication date	Feb 27, 2018
Grant date	Feb 27, 2018

Abstract

Provided are a macroporous titanium compound monolith and a production method thereof, the macroporous titanium compound monolith having a framework that is composed of a titanium compound other than titanium dioxide, having controlled macropores, and having electron conductivity, the titanium compound being oxygen-deficient titanium oxide, titanium oxynitride, or titanium nitride. Provided is a method including: placing a macroporous titanium dioxide monolith and a metal having titanium-reducing ability in a container, the macroporous titanium dioxide monolith having a co-continuous structure of a macropore and a framework that is composed of titanium dioxide; creating a vacuum atmosphere or an inert gas atmosphere within the container; and heating the monolith and the metal to cause gas-phase reduction that removes oxygen atom from the titanium dioxide composing the monolith by the metal acting as an oxygen getter, thereby obtaining a macroporous oxygen-deficient titanium oxide monolith having a co-continuous structure of the macropore and a framework that is composed of oxygen-deficient titanium oxide, the macroporous oxygen-deficient titanium oxide monolith having electron conductivity derived from the oxygen-deficient titanium oxide.

First claim

The invention claimed is:

1. A macroporous titanium compound monolith having:
a co-continuous structure of a macropore, a framework of the co-continuous structure is composed of one selected from the group consisting of:
single-phase oxygen-deficient titanium oxide, the macroporous titanium compound monolith having electron conductivity derived from the oxygen-deficient titanium oxide;
titanium oxynitride, the macroporous titanium compound monolith having electron conductivity derived from the titanium oxynitride; and
titanium nitride, the macroporous titanium compound monolith having electron conductivity derived from the titanium nitride.

2. The macroporous titanium compound monolith according to claim 1 , having an electrical resistivity of 10 3 Ω·cm or less, wherein the framework is composed of the single-phase oxygen-deficient titanium oxide.

3. The macroporous titanium compound monolith according to claim 1 ,
wherein the framework is composed of the single-phase oxygen-deficient titanium oxide, and
wherein carbon particles and/or metal particles are placed within the framework and/or on a surface of the framework.

4. The macroporous titanium compound monolith according to claim 1 , being an electrode, wherein the framework is composed of the single-phase oxygen-deficient titanium oxide.

5. The macroporous titanium compound monolith according to claim 1 , wherein the framework is composed of the titanium oxynitride.

6. The macroporous titanium compound monolith according to claim 1 , wherein the framework is composed of the titanium nitride.

7. A method for producing a macroporous titanium compound monolith, comprising:
placing a macroporous titanium dioxide monolith and a metal having titanium-reducing ability in a container, the macroporous titanium dioxide monolith having a co-continuous structure of a macropore and a framework that is composed of titanium dioxide;
creating a vacuum atmosphere or an inert gas atmosphere within the container; and
heating the monolith and the metal to cause gas-phase reduction that removes oxygen atom from the titanium dioxide composing the monolith by the metal acting as an oxygen getter, thereby obtaining a macroporous oxygen-deficient titanium oxide monolith having a co-continuous structure of the macropore and a framework that is composed of oxygen-deficient titanium oxide, the macroporous oxygen-deficient titanium oxide monolith having electron conductivity derived from the oxygen-deficient titanium oxide.

8. The method for producing a macroporous titanium compound monolith according to claim 7 , wherein the metal in the form of a foil is placed in the container.

9. The method for producing a macroporous titanium compound monolith according to claim 7 , wherein the metal is at least one selected from zirconium (Zr) and hafnium (Hf).

10. The method for producing a macroporous titanium compound monolith according to claim 9 , wherein the heating is performed at a temperature of 900 to 1300° C.

11. The method for producing a macroporous titanium compound monolith according to claim 7 , wherein the titanium dioxide composing the framework of the macroporous titanium dioxide monolith is of anatase type.

12. A method for producing a macroporous titanium compound monolith, comprising:
placing a macroporous titanium compound monolith and a metal nitride in a container, the macroporous titanium compound monolith having a co-continuous structure of a macropore and a framework that is composed of titanium dioxide or oxygen-deficient titanium oxide;
creating a vacuum atmosphere or an inert gas atmosphere within the container; and
heating the monolith and the metal nitride to cause gas-phase reduction that removes oxygen atom from, and donates nitrogen atom to, the titanium compound composing the monolith by the metal nitride acting as an oxygen getter and as a nitrogen donor, thereby obtaining a macroporous titanium oxynitride monolith having a co-continuous structure of the macropore and a framework that is composed of titanium oxynitride, the macroporous titanium oxynitride monolith having electron conductivity derived from the titanium oxynitride.

13. The method for producing a macroporous titanium compound monolith according to claim 12 , wherein the metal nitride in the form of a powder is placed in the container.

14. The method for producing a macroporous titanium compound monolith according to claim 12 , wherein the metal nitride is at least one selected from titanium nitride, zirconium nitride, and hafnium nitride.

15. The method for producing a macroporous titanium compound monolith according to claim 14 , wherein the heating is performed at a temperature of 950 to 1200° C.

16. The method for producing a macroporous titanium compound monolith according to claim 12 , wherein the metal nitride, and a macroporous titanium dioxide monolith having a co-continuous structure of the macropore and a framework that is composed of titanium dioxide, are placed in the container.

17. A method for producing a macroporous titanium compound monolith, comprising
subjecting a macroporous titanium compound monolith having a co-continuous structure of a macropore and a framework that is composed of titanium dioxide, oxygen-deficient titanium oxide, or titanium oxynitride to a heat treatment in an ammonia-containing atmosphere at a temperature equal to or higher than a thermal decomposition temperature of ammonia, so as to cause gas-phase reduction that removes oxygen atom from, and donates nitrogen atom to, the titanium compound composing the monolith, thereby obtaining a macroporous titanium nitride monolith having a co-continuous structure of the macropore and a framework that is composed of titanium nitride, the macroporous titanium nitride monolith having electron conductivity derived from the titanium nitride.

18. The method for producing a macroporous titanium compound monolith according to claim 17 , wherein the heat treatment is performed at a temperature of 1000° C. or higher.

19. The method for producing a macroporous titanium compound monolith according to claim 17 , wherein a macroporous titanium dioxide monolith having a co-continuous structure of the macropore and a framework that is composed of titanium dioxide is subjected to the heat treatment in the ammonia-containing atmosphere at the temperature equal to or higher than the thermal decomposition temperature of ammonia.

Assignees

• Japan Science & Tech Agency

Inventors

• Kageyama Hiroshi
• Nakanishi Kazuki
• Kobayashi Yoji
• Kitada Atsushi
• Hasegawa George

Classifications

• C04B41/80

  of only ceramics · CPC title

• C04B41/0072

  Heat treatment · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C04B2111/0081

  as catalysts or catalyst carriers · CPC title

• C04B2235/664

  Reductive annealing · CPC title