Method for manufacture of transition metal oxide fine particles

Patent metadata

Field	Value
Publication number	US-11420258-B2
Application number	US-201917050270-A
Country	US
Kind code	B2
Filing date	May 10, 2019
Priority date	May 11, 2018
Publication date	Aug 23, 2022
Grant date	Aug 23, 2022

Abstract

The present invention provides a method for the manufacture of transition metal oxide fine particles, the method comprising the steps of: heating a strong-alkaline aqueous solution while stirring same; adding to and dissolving in the heated strong-alkaline aqueous solution a transition metal oxide; adding a strong-acid aqueous solution to the strong alkaline aqueous solution in which the transition metal oxide is dissolved, while stirring same, thereby re-dissolving a solid generated at the interface between the strong-alkaline aqueous solution and the strong-acid aqueous solution; adjusting the pH of the mixed aqueous solution resulting from mixing the strong-alkaline aqueous solution and the strong acid aqueous solution, through adjustment of the adding rate and amount of the strong-acid aqueous solution, to precipitate transition metal oxide fine particles; and separating the transition metal oxide fine particles from the mixed aqueous solution and sequentially washing, drying, and thermally treating the separated transition metal oxide fine particles.

First claim

What is claimed is:

1. A method for manufacture of transition metal oxide fine particles, the method comprising:
heating a strong alkaline aqueous solution while stirring;
adding a transition metal oxide to the heated strong alkaline aqueous solution to dissolve the transition metal oxide in the strong alkaline aqueous solution;
adding a strong acid aqueous solution to the strong alkaline aqueous solution in which the transition metal oxide is dissolved while stirring to re-dissolve a solid material formed at an interface between the strong alkaline aqueous solution and the strong acid aqueous solution;
adjusting the pH of a mixed aqueous solution of the strong alkaline aqueous solution and the strong acid aqueous solution by controlling speed and amount of adding the strong acid aqueous solution to precipitate transition metal oxide fine particles; and
separating the transition metal oxide fine particles from the mixed aqueous solution and sequentially washing, drying, and heating the separated transition metal oxide fine particles,
wherein the transition metal oxide includes molybdenum trioxide and tungsten trioxide,
wherein the dissolving of the transition metal oxide in the strong alkaline aqueous solution is performed to sequentially dissolve molybdenum trioxide and tungsten trioxide in the strong alkaline aqueous solution.

2. The method of claim 1 , wherein water and sodium hydroxide (NaOH) are mixed in a mass ratio of 6:1 to 10:1, then heated while stirring to produce the strong alkaline aqueous solution.

3. The method of claim 2 , wherein the purity of the sodium hydroxide is greater than or equal to 99%.

4. The method of claim 1 , wherein the heating of the strong alkaline aqueous solution while stirring is performed to heat the strong alkaline aqueous solution at 60 to 105° C. while stirring at 600 rpm to 700 rpm.

5. The method of claim 1 , wherein a temperature for dissolving the tungsten trioxide in the strong alkaline aqueous solution is lower than a temperature for dissolving the molybdenum trioxide in the strong alkaline aqueous solution.

6. The method of claim 1 , wherein the purity of the molybdenum trioxide is greater than or equal to 99.5%, and the purity of the tungsten trioxide is greater than or equal to 99%.

7. The method of claim 1 , wherein the dissolving of the transition metal oxide in the strong alkaline aqueous solution is performed until the transition metal oxide is saturated.

8. The method of claim 1 , wherein the dissolving of the transition metal oxide in the strong alkaline aqueous solution is performed to heat the transition metal oxide while stirring until all of suspended solids are dissolved in the strong alkaline aqueous solution.

9. The method of claim 1 , wherein the dissolving of the transition metal oxide in the strong alkaline aqueous solution is performed to heat the strong alkaline aqueous solution while stirring until the strong alkaline aqueous solution becomes transparent.

10. The method of claim 1 , wherein the dissolving of the transition metal oxide in the strong alkaline aqueous solution is performed under the same stirring and heating temperature conditions as the heating of the strong alkaline aqueous solution while stirring.

11. The method of claim 1 , wherein the strong acid aqueous solution is composed of 60% to 75% nitric acid.

12. The method of claim 1 , wherein the re-dissolving of the solid material comprises:
adding the strong acid aqueous solution;
stopping the addition of the strong acid aqueous solution when the solid material is formed;
stirring until the solid material is re-dissolved in the mixed aqueous solution of the strong alkaline aqueous solution and the strong acid aqueous solution; and
adding the strong acid aqueous solution again when the solid material is re-dissolved in the mixed aqueous solution.

13. The method of claim 1 , wherein the precipitating of the transition metal oxide fine particles is performed to generate the transition metal oxide fine particles by adjusting the pH of the mixed aqueous solution to weakly basic.

14. The method of claim 1 , wherein the precipitating of the transition metal oxide fine particles is performed to generate the transition metal oxide fine particles by reducing the pH of the mixed aqueous solution to 7.9 to 8.1.

15. The method of claim 1 , wherein the separating of the transition metal oxide fine particles from the mixed aqueous solution is performed to filter the transition metal oxide fine particles using a membrane filter, and the washing of the separated transition metal oxide fine particles is performed with distilled water of 100 g or less.

16. The method of claim 15 , wherein the washing of the separated transition metal oxide fine particles is performed such that the transition metal oxide fine particles washed with the distilled water are additionally washed with an aqueous solution of ethanol.

17. The method of claim 1 , wherein the drying of the transition metal oxide fine particles is performed to freeze dry the transition metal oxide fine particles.

18. The method of claim 1 , wherein the drying of the transition metal oxide fine particles comprises:
primary drying the transition metal oxide fine particles at room temperature for at least 24 hours; and
second drying the primarily dried transition metal oxide fine particles in a vacuum while increasing a temperature above room temperature.

19. The method of claim 1 , wherein the heating of the transition metal oxide fine particles is performed such that the transition metal oxide fine particles separated from the mixed aqueous solution are dried and heated at a temperature of 380° C. to 450° C. for at least 30 minutes.

Assignees

• Lg Electronics Inc

Inventors

• Hong Sanghyun
• Kim Jihyun
• Lee Seojin
• Shim Sangeun
• Jung Jiyoung
• Hwang Sosan
• Kwon Yooseok

Classifications

• B22F1/142

  Thermal or thermo-mechanical treatment · CPC title

• C01G39/02 Primary

  Oxides; Hydroxides · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• B22F2304/058

  Particle size above 300 nm up to 1 micrometer · CPC title