Film formation method

Patent metadata

Field	Value
Publication number	US-12569875-B2
Application number	US-202418603868-A
Country	US
Kind code	B2
Filing date	Mar 13, 2024
Priority date	Mar 13, 2023
Publication date	Mar 10, 2026
Grant date	Mar 10, 2026

Abstract

A film formation method having an excellent mass productivity, whereby a time required for forming a film having a desired thickness is short. In the film formation method, the following steps are performed: atomizing or dropletizing a liquid containing a metal complex, the liquid being raw material solution, conveying resulting mist or droplets to a base by a carrier gas, and forming a metal oxide file on the base by thermally reacting the mist or droplets in the vicinity of the base, the metal oxide film comprising a crystalline oxide semiconductor. A metal complex is used, which shows an exothermic peak at 480° C. to 520° C. in a thermogravimetric-differential thermal analysis at a temperature increase rate of 20° C./min under an oxygen-containing atmosphere.

First claim

What is claimed is:

1 . A film formation method, the method comprising steps of:
atomizing or dropletizing a liquid containing a metal complex, the liquid being raw material solution, conveying resulting mist or droplets to a base by a carrier gas, and forming a metal oxide film on the base by thermally reacting the mist or droplets in the vicinity of the base, the metal oxide film comprising a crystalline oxide semiconductor; wherein the metal complex shows an exothermic peak at 480° C. to 520° C. in a thermogravimetric-differential thermal analysis at a temperature increase rate of 20° C./min under an oxygen-containing atmosphere.

2 . The film formation method according to claim 1 , wherein the metal complex shows a mass loss of 10% to 80% at 23° C. to 400° C. in a thermogravimetric-differential thermal analysis at a temperature increase rate of 20° C./min under an oxygen-containing atmosphere, and shows a mass loss of 3% to and 50% in association with exotherm at 400° C. to 600° C.

3 . The film formation method according to claim 1 , wherein the metal complex is at least one of a metal complex having two or more different ligands and a metal complex having same ligands and substituents.

4 . The film formation method according to claim 3 , wherein
the two or more different ligands are at least two ligands selected from a group consisting of a ligand derived from acetylacetonato, a ligand having a heterocyclic structure, and a ligand represented by following formula (1), and in following formula (1), the dotted line represents a coordinate bond, *1 represents a coordinate bond position with a metal, *2 represents a bond position with a metal, each of R 1 and R 2 independently represents an alkyl group having 1 to 6 carbon atoms, and the metal complex having the same ligands and substituents is represented by following formula (2), and in formula (2), the dotted line represents a coordinate bond, each of R 3 and R 4 independently represents hydrogen atom, a halogen atom, an alkyl group having 1 to 6 carbon atoms, a phenyl group, or a tolyl group, R 5 represents a halogen atom, a formyl group, an acetoxy group, a sulfo group, a mesyl group, a nitro group, a nitroso group, a phosphoryl group, or an alkyl group having 1 to 6 carbon atoms, and X represents a central metal

5 . The film formation method according to claim 4 , wherein a central metal coordinated in the metal complex having the two or more different ligands, and the central metal represented by X in the metal complex represented by formula (2) are each, independently a d-block metal or a Group 13 metal in the periodic table.

6 . The film formation method according to claim 5 , wherein the central metals contain a Group 9 metal in the periodic table.

7 . The film formation method according to claim 5 , wherein the central metals are iridium.

8 . The film formation method according to claim 7 , wherein the metal complex having iridium as the central metal is represented by following formula (3) or formula (4),
in following formula (3) and (4), the dotted line represents a coordinate bond, and in following formula (4), R 5 represents a halogen atom, a formyl group, an acetoxy group, a sulfo group, a mesyl group, a nitro group, a nitroso group, a phosphoryl group, or an alkyl group having 1 to 6 carbon atoms

9 . The film formation method according to claim 1 , wherein the metal complex is supplied onto a base having a corundum structure.

10 . The film formation method according to claim 9 , wherein at least a part of the base having a corundum structure comprises a crystal growth plane that contains gallium as a major component.

11 . The film formation method according to claim 1 , wherein
the raw material solution further contains gallium.

12 . The film formation method according to claim 1 , wherein
the raw material solution further contains a p type dopant.

13 . A film formation method, wherein
from a raw material solution comprising a metal complex containing a Group 9 metal in the periodic table and water, a film containing the metal is formed, and the metal complex has a water solubility of 0.01 mol/L or higher.

14 . The film formation method according to claim 13 , wherein the metal is iridium.

Assignees

• Flosfia Inc

Inventors

• Shimizu Makoto
• Shiho Hiroshi
• Ando Hiroyuki
• Tsukamoto Naoyuki
• Kato Yuji

Classifications

• C09D4/00

  Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond {; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16} · CPC title

• B05D1/005

  Spin coating · CPC title

• B05D2203/30

  Other inorganic substrates, e.g. ceramics, silicon · CPC title

• C23C16/56

  After-treatment · CPC title

• C23C16/4486

  by producing an aerosol and subsequent evaporation of the droplets or particles · CPC title