IP Library Granted Patent US 11,384,450
Granted Patent B2
US 11,384,450 · App. 16/972,997 · Granted Jul 12, 2022

Method of making thin films

Inventors: Michelle Dolgos (Corvallis, OR); Dylan Fast (Corvallis, OR); May Nyman (Corvallis, OR); Brady J. Gibbons (Corvallis, OR); Matthew O. Clark (Corvallis, OR)
Assignee: OREGON STATE UNIVERSITY
C30B29/30B05D1/005C01G33/006C30B7/04H01L41/317C01P2006/40
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Quick Facts
Patent No.
US 11,384,450
App. No.
16/972,997
Granted
Jul 12, 2022
Kind
B2
Abstract

Embodiments disclosed herein include potassium sodium niobate (KNN) films and methods of making such films. In an embodiment, a method of forming a potassium sodium niobate (KNN) film comprises preparing a solution comprising water, potassium hexaniobate salts, and sodium hexaniobate salts. In an embodiment, the solution is spin coated onto a substrate to form a film on at least a portion of a surface of the substrate. In an embodiment, the method may further comprise heat treating the film.

Claims (25)

1. A method of forming a potassium sodium niobate (KNN) film, comprising:

preparing a solution comprising:

water;

potassium hexaniobate salts; and

sodium hexaniobate salts;

spin coating the solution onto a substrate to form a film on at least a portion of a surface of the substrate; and

heat treating the film.

2. The method of claim 1 , wherein one or both of the potassium hexaniobate salts and the sodium hexaniobate salts are protonated.

3. The method of claim 2 , wherein a ratio of alkali to niobium (X:Nb, where X is potassium or sodium) of the protonated sodium hexaniobate salts and/or the protonated potassium hexaniobate salts is from about 8:6 to about 6:6.

4. The method of claim 1 , wherein a ratio of potassium hexaniobate salts to sodium hexaniobate salts in the solution is from 1.2:0.8 to 1:1.

5. The method of claim 4 , wherein the ratio of potassium hexaniobate salts to sodium hexaniobate salts in the solution is 1.14:0.86.

6. The method of claim 1 , wherein the solution further comprises one or more of lithium, silver, cesium, manganese, antimony, tantalum, bismuth, and tin compounds that are water soluble.

7. The method of claim 1 , wherein the solution further comprises hydrogen peroxide.

8. The method of claim 1 , wherein the substrate comprises Al 2 O 3 or single crystal SrTiO 3 .

9. The method of claim 1 , wherein the operations of spin coating the solution onto the substrate and heat treating the film are repeated a plurality of times.

10. The method of claim 9 , wherein the film has a thickness from about 10 nm to about 10,000 nm.

11. The method of claim 1 , wherein heat treating the film comprises annealing the film in a rapid thermal annealing system with a temperature that ranges from about 600° C. to about 1,000° C. and for a period of time that ranges from about 1 minute to about 5 minutes.

12. The method of claim 1 , wherein the potassium hexaniobate salts are prepared by:

reacting hydrated niobium oxide with potassium hydroxide; and

precipitating the potassium hexaniobate salts.

13. The method of claim 12 , wherein preparing the potassium hexaniobate salts further comprises supplying a dilute acid to dissolved potassium hexaniobate salts in order to precipitate protonated potassium hexaniobate salts.

14. The method of claim 1 , wherein the sodium hexaniobate salts are prepared by:

dissolving potassium hexaniobate salts in water with an excess of sodium hydroxide; and

precipitating the sodium hexaniobate salts.

15. The method of claim 14 , wherein preparing the sodium hexaniobate salts further comprises supplying a dilute acid to the dissolved sodium hexaniobate salts in order to precipitate protonated sodium hexaniobate salts.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jun 8, 2023
From: OREGON STATE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 063916/0051 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 17, 2021
From: DOLGOS, MICHELLE; FAST, DYLAN; NYMAN, MAY; GIBBONS, BRADY J.; CLARK, MATTHEW O.
To: OREGON STATE UNIVERSITY
Reel/Frame 055625/0644 →
Continuity (2)
Provisional Application 62684834 · Jun 14, 2018
Related Publication 20210254239A1 · Aug 19, 2021