Granted Patent B2

US 12,410,065 · App. 17/283,089 · Granted Sep 9, 2025

Inventors: Delia Milliron (Austin, TX); Gary Ong (Temecula, CA); Camila Saez Cabezas (Austin, TX); Hsin-Che Lu (Austin, TX)

Assignee: BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM

C01G33/00C09K9/00G02F1/155B82Y40/00C01P2002/77C01P2004/03C01P2004/04C01P2004/16C01P2004/64C01P2006/14C01P2006/40G02F2201/12G02F2202/36

Abstract

Claims (31)

1. A porous electrochromic niobium oxide film comprising:

a plurality of niobium oxide nanocrystals,

wherein the plurality of niobium oxide nanocrystals comprise niobium oxide having a formula NbO x where x represents an average Nb: O ratio in the niobium oxide and where x is from 2 to 2.6,

wherein the plurality of niobium oxide nanocrystals are substantially plate-shaped such that the plurality of niobium oxide nanocrystals comprise a plurality of plate-shaped niobium oxide nanocrystals, and

wherein the plurality of plate-shaped niobium oxide nanocrystals have an average length of from 0.5 nm to 200 nm, an average width of from 0.5 nm to 95 nm, and an average thickness of from 0.5 nm to 20 nm.

2. The porous electrochromic niobium oxide film of claim 1 , wherein x is from 2.3 to 2.5.

3. The porous electrochromic niobium oxide film of claim 1 , wherein the plurality of niobium oxide nanocrystals comprise Nb 2 O 5 , Nb 12 O 29 , or a combination thereof.

4. The porous electrochromic niobium oxide film of claim 1 , wherein the plurality of niobium oxide nanocrystals further comprise a plurality of rod-shaped niobium oxide nanocrystals and the plurality of rod-shaped niobium oxide nanocrystals have an average length of from 0.5 nm to 200 nm and an average width of from 0.5 nm to 20 nm.

5. The porous electrochromic niobium oxide film of claim 1 , wherein the average width and the average thickness are substantially the same, such that the plurality of plate-shaped niobium oxide nanocrystals are substantially rod-shaped.

6. The porous electrochromic niobium oxide film of claim 1 , wherein the plurality of niobium oxide nanocrystals have a crystal structure that is substantially orthorhombic, pseudo-hexagonal, substantially monoclinic, or a combination thereof.

7. The porous electrochromic niobium oxide film of claim 6 , wherein the plurality of plate-shaped niobium oxide nanocrystals have an elongated axis that is substantially parallel to the [001] direction of the crystal structure or the [011] direction of the crystal structure.

8. The porous electrochromic niobium oxide film of claim 1 , wherein the plurality of niobium oxide nanocrystals are substantially free of ligands and/or capping materials.

9. The porous electrochromic niobium oxide film of claim 1 , wherein the porous electrochromic niobium oxide film has an average porosity of from 15% to 80%.

10. The porous electrochromic niobium oxide film of claim 1 , wherein the porous electrochromic niobium oxide film has an average thickness of from 10 nm to 2 microns.

11. A method of making the porous electrochromic niobium oxide film of claim 1 , the method comprising:

making the plurality of niobium oxide nanocrystals, wherein making the niobium oxide nanocrystals comprises aminolysis-driven formation of a plurality of niobium oxo clusters, condensation of the plurality of niobium oxo clusters into a plurality of amorphous niobium oxide seeds, and crystallization and growth of the plurality of amorphous niobium oxide seeds to thereby form the plurality of niobium oxide nanocrystals;

dispersing the plurality of niobium oxide nanocrystals in a first solvent, thereby forming a dispersion; and

depositing the dispersion on a substrate;

thereby forming the electrochromic niobium oxide film.

12. The method of claim 11 , wherein the method of making the plurality of niobium oxide nanocrystals comprises:

mixing a niobium salt with a ligand and a second solvent to form a solution comprising a niobium-ligand complex;

mixing the solution comprising the niobium-ligand complex with an amine, an alcohol, or a combination thereof, and subsequently heating at a first temperature to form a solution comprising a plurality of niobium oxo clusters; and

heating the solution comprising the plurality of niobium oxo clusters at a second temperature to crystallize and grow the plurality of niobium oxide nanocrystals.

13. The method of claim 12 , wherein the niobium salt comprises a niobium halide, a niobium ethoxide, a niobium oxalate, or a combination thereof.

14. The method of claim 12 , wherein the ligand comprises an alkyl carboxylic acid, an alkylphosphonic acid, and alkylphosphinic acid, an alkylsulfonic acid, or combinations thereof.

15. The method of claim 12 , wherein the niobium-ligand complex comprises a niobium oleate complex.

16. The method of claim 12 , wherein the method is performed under an inert atmosphere.

17. The method of claim 12 , further comprising stripping the ligands from the plurality of niobium oxide nanocrystals prior to forming the electrochromic niobium oxide film.

18. An electrochromic electrode comprising the porous electrochromic niobium oxide film of claim 1 deposited on a conducting layer.

19. An electrochromic device comprising the electrochromic film of claim 1 , wherein the electrochromic device comprises an electronic device, an energy storage device, an energy conversion device, an optical device, an optoelectronic device, or a combination thereof.

20. The porous electrochromic niobium oxide film of claim 1 , wherein the average length of the plurality of plate-shaped niobium oxide nanocrystals is from 0.5 nm to 95 nm.

Assignments (1)

Continuity (2)

References Cited (136)