Method for producing hexagonal tungsten oxide and method for producing electrochromic device including the same

Patent metadata

Field	Value
Publication number	US-11873232-B2
Application number	US-202117477182-A
Country	US
Kind code	B2
Filing date	Sep 16, 2021
Priority date	Dec 1, 2020
Publication date	Jan 16, 2024
Grant date	Jan 16, 2024

Abstract

Provided is a method for producing hexagonal tungsten oxide, the method including preparing an alkaline solvent having a pH of 8 to 9, which contains at least one of water or alcohol, adding tungsten chloride to the alkaline solvent to form a first reaction solution, adding an additive to the first reaction solution to form a second reaction solution, and adding strong acid to the second reaction solution to form nanoparticles. The additive includes any one of an amine compound having 1 to 8 carbon atoms or an aliphatic hydrocarbon derivative having 10 or more carbon atoms.

First claim

What is claimed is:

1. A method for producing hexagonal tungsten oxide, the method comprising:
preparing an alkaline solvent having a pH of 8 to 9, which contains at least one of water or alcohol;
adding tungsten hexachloride (WCl 6 ) to the alkaline solvent to form a first reaction solution;
adding an additive to the first reaction solution to form a second reaction solution; and
adding strong acid to the second reaction solution to form nanoparticles,
wherein the additive includes any one of an amine compound having 1 to 8 carbon atoms or an aliphatic hydrocarbon derivative having 10 or more carbon atoms.

2. The method of claim 1 , wherein the amine compound contains at least one of urea, monoethanolamine, aniline, or octylamine.

3. The method of claim 1 , wherein the amine compound is added in an amount of about 300 mol % to about 1200 mol % of an added amount of the tungsten hexachloride.

4. The method of claim 1 , wherein the aliphatic hydrocarbon derivative contains at least one of polyethylene glycol, poly(methyl methacrylate), polyacrylamide, polyvinyl alcohol, or hexadecylamine.

5. The method of claim 1 , wherein the aliphatic hydrocarbon derivative is added in an amount of about 30 mol % to about 120 mol % of an added amount of the tungsten hexachloride.

6. The method of claim 1 , wherein the preparing of the first reaction solution, the preparing of the second reaction solution, and the adding of strong acid to the second reaction solution are performed at a temperature from 60° C. to 80° C.

7. The method of claim 1 , further comprising:
cooling the resultant mixture to room temperature after the adding of the strong acid to precipitate the nanoparticles;
separating the precipitated nanoparticles through a centrifugal separation method;
washing and drying the separated nanoparticles; and
heat treating the dried nanoparticles to form dry powder.

8. A method for producing an electrochromic device, the method comprising:
preparing an alkaline solvent having a pH of 8 to 9, which contains at least one of water or alcohol;
adding tungsten hexachloride (WCl 6 ) to the alkaline solvent to form a first reaction solution;
adding an additive to the first reaction solution to form a second reaction solution;
adding strong acid to the second reaction solution to form hexagonal tungsten oxide nanoparticles;
cooling the resultant mixture to room temperature after the adding of the strong acid to precipitate the hexagonal tungsten oxide nanoparticles;
separating the precipitated hexagonal tungsten oxide nanoparticles through a centrifugal separation method;
washing and drying the separated hexagonal tungsten oxide nanoparticles;
heat treating the dried hexagonal tungsten oxide nanoparticles to form dry powder;
mixing the dry powder with a solvent and weak acid to prepare a slurry;
applying the slurry onto a positive electrode to form a coating film;
disposing a negative electrode spaced apart from the positive electrode with the coating film therebetween; and
inserting an electrolyte between the coating film and the negative electrode, wherein the additive includes any one of an amine compound having 1 to 8 carbon atoms or an aliphatic hydrocarbon derivative having 10 or more carbon atoms.

9. The method of claim 8 , wherein the weak acid contains at least one of tetraethyoxysilane (TEOS), acetic acid, or poly(methacrylic) acid.

10. A method for producing hexagonal tungsten oxide, the method comprising:
preparing a solvent containing at least one of water or alcohol;
adding an alkali salt to the solvent to form an alkaline solvent;
adding tungsten hexachloride (WCl 6 ) to the alkaline solvent to form a first reaction solution;
adding an additive to the first reaction solution to form a second reaction solution; and
adding strong acid to the second reaction solution to form nanoparticles,
wherein the additive contains at least one of urea, monoethanolamine, or polyethylene glycol, and
the number of moles of the added strong acid is greater than the sum of the number of moles of the tungsten chloride and the number of moles of the additive.

11. The method of claim 10 , wherein the number of moles of the added strong acid is at least 1.1 times or more of the sum of the number of moles of the tungsten hexachloride and the number of moles of the additive.

12. The method of claim 10 , wherein the alkaline solvent has a pH of 8 to 9.

13. The method of claim 10 , wherein the forming of the alkaline solvent is performed at a temperature from 20° C. to 80° C.

14. The method of claim 10 , wherein the preparing of the first reaction solution, the preparing of the second reaction solution, and the adding of strong acid to the second reaction solution are performed at a temperature from 60° C. to 80° C.

15. The method of claim 10 , further comprising:
cooling the resultant mixture to room temperature after the adding of the strong acid to precipitate the nanoparticles;
separating the precipitated nanoparticles through a centrifugal separation method;
washing and drying the separated nanoparticles; and
heat treating the dried nanoparticles to form dry powder.

16. A method for producing hexagonal tungsten oxide, the method comprising:
preparing a solvent containing at least one of water or alcohol;
adding an alkali salt to the solvent to form an alkaline solvent having a pH of 8 to 9;
adding an additive to the alkaline solvent to form a first reaction solution;
adding tungsten hexachloride (WCl 6 ) to the first reaction solution to form a second reaction solution; and
adding strong acid to the second reaction solution to form nanoparticles,
wherein the additive contains at least one of urea, monoethanolamine, or polyethylene glycol, and
the preparing of the first reaction solution, the preparing of the second reaction solution, and the adding of strong acid to the second reaction solution are performed at a temperature from 60° C. to 80° C.

Assignees

• Electronics & Telecommunications Res Inst

Inventors

• Ryu Hojun
• Cho Doo-Hee
• Song Juhee
• Ah Chil Seong
• Cheon Sang Hoon

Classifications

• C01G41/02 Primary

  Oxides; Hydroxides · CPC title

• G02F1/1524

  Transition metal compounds · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• C01P2004/22

  with a polygonal circumferential shape · CPC title

• C01P2004/64

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