IP Library Granted Patent US 9,296,621
Granted Patent B2
US 9,296,621 · App. 14/229,445 · Granted Mar 29, 2016

Doping and reduction of nanostructures and thin films through flame annealing

Inventors: Yunzhe Feng (Redwood City, CA); Xiaolin Zheng (Aptos, CA); In Sun Cho (Aptos, CA)
Assignee: The Board of Trustees of the Leland Stanford Junior University
C01G9/02B01J21/063B01J23/06B01J23/22B01J27/20B01J27/22B01J35/002B01J35/004B01J35/06B01J37/16B01J37/349C01G3/02C01G23/053C01G31/00C01G49/06C23C18/125C23C18/1216C23C18/1229C23C18/1245C23C18/1254C01P2002/54C01P2004/03C01P2004/04C01P2004/16
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Quick Facts
Patent No.
US 9,296,621
App. No.
14/229,445
Granted
Mar 29, 2016
Kind
B2
Abstract

A sol-flame method includes 1) forming a sol-gel precursor solution of a source of a dopant; 2) coating a nanostructure or a thin film with the sol-gel precursor solution; and 3) subjecting the coated nanostructure or the coated thin film to flame annealing to form a doped nanostructure or a doped thin film.

Claims (23)

1. A sol-flame method, comprising:

forming a sol-gel precursor solution of a source of a dopant;

coating a nanostructure or a thin film with the sol-gel precursor solution; and

subjecting the coated nanostructure or the coated thin film to flame annealing to form a doped nanostructure or a doped thin film,

wherein a concentration of the dopant at a surface of the doped nanostructure or the doped thin film is at least 5 at. %, and a concentration of the dopant at a depth of 10 nm below the surface is at least 50% of the concentration of the dopant at the surface.

2. The sol-flame method of claim 1 , wherein the dopant is a metal or a metalloid.

3. The sol-flame method of claim 1 , wherein the sol-gel precursor solution includes a salt of the dopant at a concentration in the range of 0.01 M to 0.2 M.

4. The sol-flame method of claim 1 , wherein coating with the sol-gel precursor solution is carried out by dip-coating or spin-coating.

5. The sol-flame method of claim 1 , wherein flame annealing is carried out at a temperature in the range of 900° C. to 1400° C.

6. The sol-flame method of claim 1 , wherein flame annealing is carried out for a duration in the range of 5 s to 5 min.

7. The sol-flame method of claim 1 , wherein flame annealing is carried out at a heating rate of at least 50° C./s.

8. The sol-flame method of claim 1 , wherein flame annealing is carried out at a fuel-to-oxidizer equivalence ratio up to 1.1.

9. The sol-flame method of claim 1 , wherein flame annealing is carried out at a fuel-to-oxidizer equivalence ratio up to 1.

10. The sol-flame method of claim 1 , wherein the dopant is a first dopant, and further comprising annealing the doped nanostructure or the doped thin film in the presence of a gaseous source of a second dopant to form a codoped nanostructure or a codoped thin film.

11. The sol-flame method of claim 1 , wherein the dopant is a first dopant, the sol-gel precursor solution includes a source of a second dopant, and flame annealing is carried out to form a codoped nanostructure or a codoped thin film.

12. A flame reduction method, comprising:

providing a nanostructure or a thin film; and

subjecting the nanostructure or the thin film to flame annealing to introduce oxygen vacancies in the nanostructure or the thin film wherein the reactivity of the nanostructure or the thin film is increased,

wherein flame annealing is carried out at a temperature of at least 900° C., and a fuel-to-oxidizer equivalence ratio that is greater than 1.

13. The flame reduction method of claim 12 , wherein flame annealing is carried out at the temperature of at least 900° C. for a duration in the range of 5 s to 5 min.

14. The flame reduction method of claim 12 , wherein the fuel-to-oxidizer equivalence ratio is greater than 1 and is up to 1.5.

15. The flame reduction method of claim 12 , wherein flame annealing is carried out with a partial pressure of O 2 that is less than 0.4 Pa.

16. The flame reduction method of claim 12 , wherein the nanostructure or the thin film includes a metal oxide, and an oxygen-to-metal molar ratio at a surface of the nanostructure or the thin film subsequent to flame annealing is no greater than 80% of an initial oxygen-to-metal molar ratio at the surface prior to flame annealing.

Assignments (2)
CONFIRMATORY LICENSE Recorded Oct 6, 2017
From: STANFORD UNIVERSITY
To: NAVY, SECRETARY OF THE UNITED STATES OF AMERICA
Reel/Frame 044235/0394 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 19, 2016
From: FENG, YUNZHE; ZHENG, XIAOLIN; CHO, IN SUN
To: THE BOARD OF TRUSTEES OF THE LELAND STANFORD JUNIOR UNIVERSITY
Reel/Frame 037773/0858 →
Continuity (2)
Provisional Application 61806728 · Mar 29, 2013
Related Publication 20140294721A1 · Oct 2, 2014