Microwave assisted and low-temperature fabrication of nanowire arrays on scalable 2D and 3D substrates

Patent metadata

Field	Value
Publication number	US-11465129-B2
Application number	US-201816465969-A
Country	US
Kind code	B2
Filing date	Jun 1, 2018
Priority date	Jun 6, 2017
Publication date	Oct 11, 2022
Grant date	Oct 11, 2022

Abstract

A method of making a titanium dioxide nanowire array includes contacting a substrate with a solvent comprising a titanium (III) precursor, an acid, and an oxidant while microwave heating the solvent, thereby forming a hydrogen titanate H2Ti2O5.H2O nanowire array. The hydrogen titanate nanowire array is annealed to form a titanium dioxide nanowire array. The substrate is seeded with titanium dioxide before starting the hydrothermal synthesis of the hydrogen titanate nanowire array. The titanium dioxide nanowire array is loaded with a platinum group metal to form an exhaust gas catalyst. The titanium dioxide nanowire array can be used to catalyze oxidation of combustion exhaust.

First claim

What is claimed is:

1. A method of making a hydrogen titanate nanowire array, the method comprising: contacting a substrate with a solvent comprising a titanium (III) precursor, an acid, and an oxidant while microwave heating the solvent, thereby forming a hydrogen titanate nanowire array.

2. The method of claim 1 , wherein the substrate comprises a cordierite honeycomb monolith.

3. The method of claim 1 , wherein the solvent is a polar solvent.

4. The method of claim 1 , wherein the solvent is a protic solvent.

5. The method of claim 1 , wherein the solvent is water.

6. The method of claim 1 , wherein the titanium (III) precursor is TiCl 3 .

7. The method of claim 1 , wherein the titanium (III) precursor is Ti 2 (SO 4 ) 3 .

8. The method of claim 1 , wherein the titanium (III) precursor is a titanium (III) alkoxide.

9. The method of claim 1 , wherein the acid is hydrochloric acid (HCl).

10. The method of claim 9 , wherein the acid is from about 25 wt. % to about 40 wt. % HCl.

11. The method of claim 1 , wherein the acid is sulfuric acid (H 2 SO 4 ).

12. The method of claim 1 , wherein the oxidant is hydrogen peroxide.

13. The method of claim 12 , wherein the hydrogen peroxide is from about 20 wt. % to about 40 wt. % in water.

14. The method of claim 1 , wherein the solvent is heated by microwave heating to a temperature from about 75° C. to about 95° C.

15. The method of claim 1 , wherein the solvent is heated by microwave heating for a duration from about 10 minutes to about 180 minutes.

16. The method of claim 1 , further comprising annealing the hydrogen titanate nanowire array to form a TiO2 nanowire array.

17. The method of claim 16 , wherein annealing is performed at a temperature from about 300° C. to about 800° C.

18. The method of claim 1 , wherein the solvent is a second solvent, the method further comprising contacting the substrate with a first solvent comprising a titanium (IV) precursor and a first acid prior to contacting the substrate with the second solvent.

19. The method of claim 18 , further comprising sonicating while contacting the substrate with the first solvent.

20. The method of claim 18 , wherein the titanium (IV) precursor comprises one or more of titanium (IV) isopropoxide, titanium (IV) n-butoxide, and titanium (IV) chloride.

21. The method of claim 20 , wherein the titanium (IV) precursor comprises titanium (IV) isopropoxide.

22. The method of claim 18 , wherein the first solvent is a polar solvent.

23. The method of claim 18 , wherein the first solvent is a protic solvent.

24. The method of claim 18 , wherein the first solvent is an alcohol.

25. The method of claim 18 , wherein the first solvent is ethanol.

26. The method of claim 18 , wherein the first acid is HNO 3 .

27. The method of claim 18 , further comprising drying the substrate after contacting the substrate with the first solvent, and subsequently contacting the substrate with the first solvent prior to contacting the substrate with the second solvent.

28. The method of claim 18 , further comprising annealing the substrate after contacting the substrate with the first solvent and prior to contacting the substrate with the second solvent.

29. The method of claim 16 , further comprising loading a platinum group metal onto the titanium dioxide (TiO 2 ) nanowire array, the method further comprising:
contacting the TiO 2 nanowire array with a third solvent comprising a platinum group metal precursor, wherein the platinum group metal precursor comprises one or more of platinum, palladium, and rhodium;
drying the TiO 2 nanowire array;
calcining the TiO 2 nanowire array; and
annealing the TiO 2 nanowire array in the presence of hydrogen.

30. The method of claim 29 , wherein the platinum group metal precursor comprises platinum.

31. The method of claim 30 , where the platinum is platinum (II).

32. The method of claim 29 , wherein the platinum group metal precursor comprises tetraammineplatinum (II) nitrate.

33. The method of claim 29 , further comprising sonicating while contacting the TiO 2 nanowire array with the third solvent.

34. The method of claim 29 , further comprising contacting the TiO 2 nanowire array with a third solvent, drying the TiO 2 nanowire array, and calcining the TiO 2 nanowire array a plurality of times prior to annealing the TiO 2 nanowire array.

35. The method of claim 1 , wherein the hydrogen titanate nanowire array comprises H 2 Ti 2 O 5 .H 2 O.

Assignees

• Univ Connecticut

Inventors

• Gao Pu-Xian
• Lu Xingxu
• Hoang Son

Classifications

• C04B35/62259

  Fibres based on titanium oxide · CPC title

• B01D53/864

  Removing carbon monoxide or hydrocarbons · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• B01D53/8628

  Processes characterised by a specific catalyst · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title