IP Library Granted Patent US 12679741
Granted Patent B2
US 12679741 · App. 18/040,687 · Granted Jul 14, 2026

Aerosol-assisted synthesis of crystalline tungsten bronze particles

Inventors: Daren Chen (Glen Allen, VA); Hao Tu (Henrico, VA)
Assignee: Virginia Commonwealth University
C01G41/006C01P2002/72C01P2004/03
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Quick Facts
Patent No.
US 12679741
App. No.
18/040,687
Granted
Jul 14, 2026
Kind
B2
Abstract

Provided herein are methods for producing crystalline tungsten bronze oxide particles. The method may include atomizing a liquid solution comprising an alkali metal precursor and a tungsten precursor to produce droplets; mixing the droplets with one or more gaseous flows to produce a combined flow; flowing the combined flow through a heated reactor to provide crystalline tungsten bronze oxide particles having the formula M x WO 3 , wherein M is the alkali metal; and collecting the particles.

Claims (30)

1 . A method for producing crystalline tungsten bronze oxide particles, comprising

atomizing a liquid solution comprising an alkali metal precursor and a tungsten precursor to produce droplets, wherein a molar ratio of alkali metal precursor to tungsten precursor is from 0.4:1 to 1:1;

mixing the droplets with one or more gaseous flows to produce a combined flow;

flowing the combined flow through a heated reactor to provide crystalline tungsten bronze oxide particles having the formula M x WO 3 , wherein M is the alkali metal and x is a number from zero to 1; and

collecting the particles.

2 . The method of claim 1 , wherein the particles are collected using baghouse filter sampling, a cyclone, an impactor, a thermo-precipitator, or electrostatic sampling.

3 . The method of claim 1 , wherein the tungsten precursor is ammonium tungstate or tungsten chloride.

4 . The method of claim 1 , wherein the alkali metal is selected from sodium, potassium, and cesium.

5 . The method of claim 1 , wherein the one or more gaseous flows comprise nitrogen and hydrogen.

6 . The method of claim 1 , wherein a flow rate through the reactor is 0.1-15 SLPM.

7 . The method of claim 1 , wherein the reactor comprises a plurality of tube reactors.

8 . The method of claim 1 , wherein the reactor comprises a spiral flow channel.

9 . The method of claim 1 , wherein the reactor is heated to a temperature of 600-1000° C.

10 . A method for producing crystalline tungsten bronze oxide particles, comprising

atomizing a liquid solution comprising an alkali metal precursor and a tungsten precursor to produce droplets;

mixing the droplets with one or more gaseous flows to produce a combined flow;

flowing the combined flow through a heated reactor to provide crystalline tungsten bronze oxide particles having the formula M x WO 3 , wherein M is the alkali metal and x is a number from zero to 1; and

collecting the particles, wherein the particles are in the cubic phase or tetragonal phase.

11 . The method of claim 1 , further comprising recirculating a gaseous flow after the particles are collected.

12 . The method of claim 1 , wherein the liquid solution is an aqueous solution and does not contain an organic solvent.

13 . The method of claim 1 , wherein the method does not include an annealing step.

14 . A method for producing crystalline tungsten bronze oxide particles, comprising

atomizing a liquid solution comprising an alkali metal precursor and a tungsten precursor to produce droplets;

mixing the droplets with one or more gaseous flows to produce a combined flow;

flowing the combined flow through a heated reactor to provide crystalline tungsten bronze oxide particles having the formula M x WO 3 , wherein M is the alkali metal and x is a number from zero to 1;

introducing a dilution flow to the combined flow flowing through the reactor; and

collecting the particles.

15 . The method of claim 14 , wherein a ratio of a flow rate of the dilution flow to a flow rate of the combined flow is from 2:1 to 10:1.

16 . The method of claim 14 , wherein the dilution flow is heated.

17 . The method of claim 14 , wherein the dilution flow is unheated.