IP Library Granted Patent US 11,597,658
Granted Patent B2
US 11,597,658 · App. 17/112,228 · Granted Mar 7, 2023

Preparation of nanosized cubic lithium lanthanum zirconate fast ion conductor via facile polymer-chelate combustion route

Inventors: Jon Mark Weller (Phoenix, AZ); Candace Chan (Phoenix, AZ)
Assignee: Arizona Board of Regents on behalf of Arizona State University
C01G25/006H01M4/485C01P2002/52C01P2002/72C01P2002/74C01P2002/76C01P2004/03C01P2004/04C01P2006/40C01P2006/80H01M10/0562H01M2300/0071
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Quick Facts
Patent No.
US 11,597,658
App. No.
17/112,228
Granted
Mar 7, 2023
Kind
B2
Abstract

Nanosized cubic lithium lanthanum zirconate is synthesized by forming a solution including an organic compound and compounds of lithium, lanthanum, and zirconium; drying the solution to yield a solid; and heating the solid in the presence of oxygen to pyrolyze the organic compound to yield a product comprising nanosized cubic lithium lanthanum zirconate.

Claims (34)

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

forming a solution comprising an organic compound and compounds of lithium, lanthanum, and zirconium, wherein the organic compound is poly(vinyl alcohol);

heating the solution to yield a solid; and

calcining the solid in the presence of oxygen to pyrolyze the organic compound to yield a product comprising cubic lithium lanthanum zirconate nanoparticles, wherein heating the solution comprises drying the solution above 150° C.

2. The method of claim 1 , wherein calcining the solid comprises forming a carbonaceous foam comprising the poly(vinyl alcohol) or a degradation product thereof.

3. The method of claim 2 , wherein calcining the solid comprises distributing lithium, lanthanum, and zirconium throughout the carbonaceous foam.

4. The method of claim 1 , wherein the solution comprises lithium, lanthanum, and zirconium in a molar ratio of about 10:3:2.

5. The method of claim 1 , wherein the solution comprises lithium, lanthanum, and zirconium in a molar ratio of about 10.5:3:2.

6. The method of claim 1 , wherein the compounds of lithium, lanthanum, and zirconium are nitrate salts.

7. The method of claim 1 , wherein the compounds of lithium, lanthanum, and zirconium include organic moieties.

8. The method of claim 7 , wherein the compounds of lithium, lanthanum, and zirconium include acetylacetonate.

9. The method of claim 1 , wherein the solution is aqueous or non-aqueous.

10. The method of claim 9 , wherein the solution further comprises an organic solvent.

11. The method of claim 10 , wherein the organic solvent comprises propionic acid or dichloromethane.

12. The method of claim 1 , wherein the product comprises at least 90 wt % of the cubic lithium lanthanum zirconate nanoparticles.

13. The method of claim 1 , wherein the product comprises a total amount of lanthanum zirconate, lanthanum oxide, and lithium zirconate of less than 5 wt %.

14. The method of claim 1 , wherein the product comprises less than 5 wt % of tetragonal lithium lanthanum zirconate.

15. The method of claim 1 , wherein the solution further comprises acetic acid.

16. The method of claim 1 , wherein the solution further comprises an additional metal.

17. The method of claim 16 , wherein the additional metal comprises a transition metal.

18. The method of claim 16 , wherein the additional metal comprises aluminum.

19. The method of claim 16 , wherein the additional metal comprises an alkali metal.

20. The method of claim 1 , wherein heating the solution occurs under reduced pressure, under an inert atmosphere, or both.

21. The method of claim 1 , wherein synthesizing the cubic lithium lanthanum zirconate nanoparticles occurs in the absence of gellation.

22. A method of synthesizing cubic lithium lanthanum zirconate nanoparticles, the method comprising:

forming a solution comprising an organic compound and compounds of lithium, lanthanum, and zirconium, wherein the organic compound is poly(vinyl alcohol),

heating the solution to yield a solid, and

calcining the solid in the presence of oxygen to pyrolyze the organic compound to yield a product comprising cubic lithium lanthanum zirconate nanoparticles,

wherein heating the solution comprises heating to a temperature in a range of room temperature to 250° C. for a length of time in a range of 1 to 24 hours.

23. A method of synthesizing cubic lithium lanthanum zirconate nanoparticles, the method comprising:

forming a solution comprising an organic compound and compounds of lithium, lanthanum, and zirconium, wherein the organic compound is poly(vinyl alcohol),

heating the solution to yield a solid, and

calcining the solid in the presence of oxygen to pyrolyze the organic compound to yield a product comprising cubic lithium lanthanum zirconate nanoparticles,

wherein heating the solution comprises ramping a temperature of the solution to 130° C.

Assignments (2)
CONFIRMATORY LICENSE Recorded Feb 12, 2025
From: ARIZONA STATE UNIVERSITY-TEMPE CAMPUS
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 070191/0217 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 15, 2021
From: WELLER, JON MARK; CHAN, CANDACE
To: ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY
Reel/Frame 055933/0450 →
Continuity (3)
Continuation 16009518 · Jun 15, 2018
Provisional Application 62521051 · Jun 16, 2017
Related Publication 20210230013A1 · Jul 29, 2021
Cited By (1)
US 12,227,427