Method for producing metal oxide dispersion liquid and method for producing infrared-radiation-shielding film

Patent metadata

Field	Value
Publication number	US-11535523-B2
Application number	US-201916770964-A
Country	US
Kind code	B2
Filing date	Feb 7, 2019
Priority date	Feb 14, 2018
Publication date	Dec 27, 2022
Grant date	Dec 27, 2022

Abstract

According to this method, a fatty acid of CnH2nO2 (n=5 to 14) is mixed with a plurality of metal sources selected from Zn, In, Sn, Sb, and Al, thereby fatty acid metal salts are obtained, subsequently the fatty acid metal salts are heated at 130° C. to 250° C., and a metal soap that is a precursor is obtained. This precursor is heated at 200° C. to 350° C., and metal oxide primary particles are dispersed in the precursor melt. To this dispersion liquid, a washing solvent having a δP value higher by 5 to 12 than the δP value of the Hansen solubility parameter of the final dispersing solvent is added, thereby the metal oxide primary particles are washed and agglomerated, metal oxide secondary particles are obtained, and then washing is repeated.

First claim

What is claimed is:

1. A method for producing a dispersion liquid in which metal oxide secondary particles formed by metal oxide primary particles agglomerated together are dispersed in a hydrophobic solvent as a final dispersing solvent, the method comprising:
(a) a step of mixing, by a direct method or a metathesis method, a fatty acid of C n H 2n O 2 (n=5 to 14) with each of metal sources including a plurality of kinds of metals selected from the group consisting of Zn, In, Sn, Sb, and Al, metal oxides of the metals, metal hydroxides of the metals, and thereby obtaining a mixture of a plurality of kinds of fatty acid metal salts;
(b) a step of heating the mixture of fatty acid metal salts at a temperature of 130° C. to 250° C., subsequently cooling the mixture, and thereby obtaining a metal soap, which is a precursor of the metal oxide primary particles;
(c) a step of heating the precursor of the metal oxide primary particles at a temperature of 200° C. to 350° C., and thereby dispersing the metal oxide primary particles in a melt of the precursor;
(d) a step of adding a washing solvent that has, when a polarization term of Hansen solubility parameter (HSP) of the solvent is designated as δP, a δP value higher by 5 to 12 than the δP value of the final dispersing solvent, to the metal oxide primary particles dispersed in the melt, thereby washing the metal oxide primary particles while simultaneously causing the metal oxide primary particles to agglomerate, and thereby obtaining metal oxide secondary particles in the washing solvent;
(e) a step of removing the washing solvent present in the dispersion liquid of the metal oxide secondary particles;
(f) a step of repeating the step (d) and step (e) once or twice or more; and
(g) a step of adding, after the step (f), a hydrophobic solvent as the final dispersing solvent to the metal oxide secondary particles from which the washing solvent has been removed, and dispersing the metal oxide secondary particles having an average particle size of 50 nm to 150 nm in the hydrophobic solvent.

2. The production method according to claim 1 , wherein between the step (a) and the step (b), or between the step (b) and the step (c), a high-boiling-point solvent is added to the mixture of fatty acid metal salts or to the precursor of the metal oxide primary particles.

3. The production method according to claim 1 , wherein the metal oxide of the metal oxide primary particles and the metal oxide secondary particles is at least one kind of tin-doped indium oxide (ITO), antimony-doped tin oxide (ATO), antimony-doped zinc oxide (AZO), and aluminum-doped zinc oxide (AlZO).

4. The method for producing an infrared-radiation shielding-film by applying the dispersion liquid produced by the method according to claim 1 on a base material and thereby forming an infrared-radiation-shielding film.

5. The production method according to claim 2 , wherein the metal oxide of the metal oxide primary particles and the metal oxide secondary particles is at least one kind of tin-doped indium oxide (ITO), antimony-doped tin oxide (ATO), antimony-doped zinc oxide (AZO), and aluminum-doped zinc oxide (AlZO).

6. The method for producing an infrared-radiation shielding-film by applying the dispersion liquid produced by the method according to claim 2 on a base material and thereby forming an infrared-radiation-shielding film.

7. The method for producing an infrared-radiation shielding-film by applying the dispersion liquid produced by the method according to claim 3 on a base material and thereby forming an infrared-radiation-shielding film.

8. The method for producing an infrared-radiation shielding-film by applying the dispersion liquid produced by the method according to claim 5 on a base material and thereby forming an infrared-radiation-shielding film.

Assignees

• Mitsubishi Materials Corp

Inventors

• Higano Satoko

Classifications

• C01G19/02 Primary

  Oxides · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C09K3/00

  Materials not provided for elsewhere · CPC title

• C01G15/00

  Compounds of gallium, indium or thallium · CPC title

• C01P2004/50

  Agglomerated particles · CPC title