Methods for forming crystalline metal oxide over structural color film using low heat

Patent metadata

Field	Value
Publication number	US-10882996-B2
Application number	US-201916258065-A
Country	US
Kind code	B2
Filing date	Jan 25, 2019
Priority date	Jun 29, 2018
Publication date	Jan 5, 2021
Grant date	Jan 5, 2021

Abstract

A method for forming a multilayer thin film having a crystalline metal oxide layer, the method including: encapsulating at least one encapsulated layer of the multilayer thin film in a wet chemical composition by wet chemical methods; and crystallizing the wet chemical composition by microwave hydrothermal treatment to form a crystalline metal oxide layer encapsulating the at least one encapsulated layer of the multilayer thin film.

First claim

What is claimed is:

1. A method for forming a multilayer thin film comprising a crystalline metal oxide layer, the method comprising:
encapsulating at least one encapsulated layer of the multilayer thin film in a wet chemical composition by wet chemical methods; and
crystallizing the wet chemical composition by microwave hydrothermal treatment to form a crystalline metal oxide layer encapsulating the at least one encapsulated layer of the multilayer thin film,
wherein the multilayer thin film produces an omnidirectional structural color.

2. The method of claim 1 , wherein the at least one encapsulated layer of the multilayer thin film is a reflective core layer, and the crystalline metal oxide layer encapsulates the reflective core layer.

3. The method of claim 2 , wherein the reflective core layer comprises Al, Ag, Pt, Sn, Au, Cu, brass, TiN, Cr, or a combination thereof, and
the crystalline metal oxide layer comprises SnO 2 , ZrO 2 , CeO 2 , Co 3 O 4 , Co 2 O 3 , Fe 2 O 3 , Fe 3 O 4 or TiO 2 .

4. The method of claim 1 , wherein the multilayer thin film comprises:
a reflective core layer;
a first layer extending across the reflective core layer;
a second layer extending across the first layer; and
the crystalline metal oxide layer encapsulating the second layer, the first layer, and the reflective core layer.

5. The method of claim 4 , wherein
the reflective core layer comprises Al, Ag, Pt, Sn, Au, Cu, brass, TiN, Cr, or a combination thereof,
the first layer comprises at least one a dielectric material or at least one dielectric absorbing material,
the second layer comprises a semi-transparent absorbing material, and
the crystalline metal oxide layer comprises Fe 2 O 3 or TiO 2 .

6. The method of claim 4 , wherein the multilayer thin film further comprises a protective layer encompassing the reflective core layer and the protective layer is present between the reflective core layer and the first layer.

7. The method of claim 6 , wherein
the reflective core layer comprises Al, Ag, Pt, Sn, Au, Cu, brass, TiN, Cr, or a combination thereof,
the protective layer comprises SiO 2 , Al 2 O 3 , ZrO 2 , or CeO 2 ,
the first layer comprises at least one a dielectric material or at least one dielectric absorbing material,
the second layer comprises a semi-transparent absorbing material, and
the crystalline metal oxide layer comprises Fe 2 O 3 or TiO 2 .

8. The method of claim 6 , wherein the protective layer is formed by encapsulating the reflective core layer in a second wet chemical composition by wet chemical methods, wherein the second wet chemical composition is different from the wet chemical composition; and
crystallizing the second wet chemical composition by microwave hydrothermal treatment to form a second crystalline metal oxide layer encapsulating the reflective core layer.

9. The method of claim 1 , wherein the wet chemical composition is crystallized by heating the wet chemical composition to a temperature from 150° C. to 300° C.

10. The method of claim 9 , wherein the crystalline metal oxide layer comprises TiO 2 that was crystallized by heating the wet chemical composition to a temperature from 150° C. to 200° C. to form a crystalline TiO 2 layer.

11. The method of claim 10 , wherein the crystalline TiO 2 layer comprises anatase phase TiO 2 .

12. The method of claim 9 , wherein the crystalline metal oxide layer comprises Fe 2 O 3 and was crystallized by heating the wet chemical composition to a temperature from 150° C. to 250° C. to form a crystalline Fe 2 O 3 layer.

13. The method of claim 12 , wherein the crystalline Fe 2 O 3 layer comprises α-Fe 2 O 3 .

14. The method of claim 1 , wherein the wet chemical composition is crystallized in a microwave reactor, and
a pressure within the microwave reactor during a crystallization of the wet chemical composition is from 10 bar to 30 bar.

15. The method of claim 1 , wherein the crystalline metal oxide layer has a thickness from greater than 0 nm to 250 nm.

16. The method of claim 1 , wherein the crystalline metal oxide layer has a surface roughness (Ra) of less than 100 nm.

17. A method forming a multilayer thin film comprising a reflective core layer, a crystalline metal oxide layer encapsulating the reflective core layer, a first layer extending across the crystalline metal oxide layer, and a second layer extending across the first layer, wherein:
the crystalline metal oxide layer is formed by:
encapsulating the reflective core layer in a wet chemical composition by wet chemical methods; and
crystallizing the wet chemical composition by microwave hydrothermal treatment to form a crystalline metal oxide layer encapsulating the reflective core layer; and

the multilayer thin film produces an omnidirectional structural color.

18. The method of claim 17 , wherein
the reflective core layer comprises Al, Ag, Pt, Sn, Au, Cu, brass, TiN, Cr, or a combination thereof,
the crystalline metal oxide layer comprises Fe 2 O 3 ;
the first layer comprises a semi-transparent absorbing material, and
the second layer comprises at least one dielectric material or at least one dielectric absorbing material.

19. The method of claim 18 , wherein the microwave hydrothermal treatment is conducted to heat the wet chemical composition to temperature from 150° C. to 250° C.

20. The method of claim 18 , wherein the crystalline metal oxide layer has a surface roughness (Ra) less than 100 nm.

Assignees

• Toyota Eng & Mfg North America
• Toyota Motor Engineering & Mfg North Amercia Inc

Inventors

• Wu Songtao
• Banerjee Debasish
• Jia Hongfei
• Gunugunuri Krishna Reddy

Classifications

• C09C1/0033 Primary

  consisting of a metal or an alloy · CPC title

• C09C2200/307

  Thickness of an outermost protective layer · CPC title

• C09C1/0078

  Pigments consisting of flaky, non-metallic substrates, characterised by a surface-region containing free metal · CPC title

• C09C1/006

  consisting of a metal or an alloy · CPC title

• C09C1/0015 Primary

  Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings · CPC title