IP Library › Granted Patent US 11,053,134
Granted Patent B2
US 11,053,134 · App. 16/111,939 · Granted Jul 6, 2021

Synthesis of nanosized cubic lithium lanthanum zirconate fast ion conductor

Inventors: Jon Mark Weller (Phoenix, AZ); Candace Chan (Phoenix, AZ)
Assignee: Arizona Board of Regents on behalf of Arizona State University
C01G25/006H01M10/0525H01M10/0562C01P2002/72C01P2002/74C01P2002/76C01P2002/85C01P2004/04C01P2004/51C01P2004/62C01P2004/64C01P2006/40H01M2300/0077
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Quick Facts
Patent No.
US 11,053,134
App. No.
16/111,939
Granted
Jul 6, 2021
Kind
B2
Abstract

Synthesizing lithium lanthanum zirconate includes combining a reagent composition with a salt composition to yield a molten salt reaction medium, wherein the reagent composition comprises a lithium component, a lanthanum component, and zirconium component having a lithium:lanthanum:zirconium molar ratio of about 7:3:2; heating the molten salt reaction medium to yield a reaction product; and washing the reaction product to yield a crystalline powder comprising lithium lanthanum zirconate.

Claims (29)

1. A method of synthesizing lithium lanthanum zirconate, the method comprising:

combining a reagent composition with a salt composition to yield a salt reaction medium, wherein the reagent composition comprises a lithium component, a lanthanum component, and zirconium component having a lithium:lanthanum:zirconium molar ratio of about 7:3:2;

heating the salt reaction medium to yield a reaction product; and

washing the reaction product to yield a crystalline powder comprising lithium lanthanum zirconate,

wherein the salt composition is selected from the group consisting of one of the following mixtures:

a eutectic mixture of potassium chloride and lithium chloride,

a eutectic mixture of lithium carbonate, sodium carbonate, and potassium carbonate,

a eutectic mixture of lithium chloride and lithium hydroxide,

a eutectic mixture of lithium bromide and potassium bromide, and

a basic mixture of lithium nitrate, lithium peroxide, and lithium hydroxide in a molar ratio of 1:2:2.

2. The method of claim 1 , wherein the lithium component comprises lithium nitrate, lithium hypochlorite, or both.

3. The method of claim 1 , wherein the lanthanum component comprises lanthanum nitrate, lanthanum oxychloride, or both.

4. The method of claim 1 , wherein the zirconium component comprises zirconium oxide, zirconium oxynitrate, or both.

5. The method of claim 1 , wherein the molten salt reaction medium comprises an extrinsic dopant.

6. The method of claim 5 , wherein the extrinsic dopant comprises aluminum, gallium, tantalum, tungsten, or any combination thereof.

7. The method of claim 1 , wherein the salt reaction medium comprises a reagent composition: salt composition weight ratio of 1:1.

8. The method of claim 1 , wherein the lithium lanthanum zirconate consists of cubic phase Li 7 La 3 Zr 2 O 12 .

9. The method of claim 1 , wherein the lithium lanthanum zirconate consists essentially of cubic phase Li 7 La 3 Zr 2 O 12 .

10. The method of claim 1 , wherein the lithium lanthanum zirconate is in the form of nanoparticles.

11. The method of claim 10 , wherein a maximum dimension of the nanoparticles is less than 1000 nm.

12. The method of claim 11 , wherein the maximum dimension of the nanoparticles is between 300 nm and 500 nm.

13. The method of claim 1 , wherein heating the molten salt reaction medium comprises heating to a temperature in a range of 700° C. to 1000° C.

14. The method of claim 1 , wherein heating the molten salt reaction medium comprises heating for a length of time up to 12 hours.

15. The method of claim 1 , further comprising combining sodium fluoride with the salt reaction mixture.

16. The method of claim 1 , wherein the zirconium component comprises zirconium oxide nanoparticles.

17. The method of claim 1 , wherein combining the reagent composition with the salt composition to yield the salt reaction medium comprises forming a mixture comprising the reagent composition and the salt composition and melting the mixture to yield the salt reaction medium.

18. The method of claim 1 , wherein the salt composition is a molten salt composition.

19. The method of claim 18 , further comprising melting the salt composition to yield the molten salt composition.

20. The method of claim 19 , wherein heating the salt reaction medium comprises heating to a temperature in a range of 500° C. to 600° C.

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 5, 2018
From: ARIZONA STATE UNIVERSITY, TEMPE
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 047420/0570 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 25, 2018
From: WELLER, JON MARK; CHAN, CANDACE
To: ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY
Reel/Frame 046963/0489 →
Continuity (2)
Provisional Application 62550155 · Aug 25, 2017
Related Publication 20190062176A1 · Feb 28, 2019
Cited By (1)
US 12,304,832