IP Library › Granted Patent US 12,304,832
Granted Patent B2
US 12,304,832 · App. 18/449,209 · Granted May 20, 2025

Synthesis of lithium lanthanum zirconate from nanocrystalline lanthanum zirconate

Inventors: Jon Weller (Phoenix, AZ); Candace Chan (Phoenix, AZ)
Assignee: Arizona Board of Regents on behalf of Arizona State University
C01G25/006C08K5/053C08K5/09C08L29/14C08L33/08C08L33/10B82Y40/00C01P2002/52C01P2002/60C01P2002/72C01P2004/03C01P2004/04
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Quick Facts
Patent No.
US 12,304,832
App. No.
18/449,209
Granted
May 20, 2025
Kind
B2
Abstract

Fabricating a layer including lithium lanthanum zirconate (Li 7 La 3 Zr 2 O 12 ) layer includes forming a slurry including lanthanum zirconate (La 2 Zr 2 O 7 ) nanocrystals, a lithium precursor, and a lanthanum precursor in stoichiometric amounts to yield a dispersion including lithium, lanthanum, and zirconium. In some cases, the dispersion includes lithium, lanthanum, and zirconium in a molar ratio of 7:3:2. In certain cases, the slurry includes excess lithium. The slurry is dispensed onto a substrate and dried. The dried slurry is calcined to yield the layer including lithium lanthanum zirconate.

Claims (19)

1. A method of synthesizing a tantalum-doped lithium lanthanum zirconate, the method comprising:

combining nanocrystals comprising a tantalum-doped lanthanum zirconate with LiNO 3 , LiOH, and Li 2 O 2 to yield a mixture; and

heating the mixture to yield the tantalum-doped lithium lanthanum zirconate,

wherein the tantalum-doped lanthanum zirconate comprises La 2.4 Zr 1.12 Ta 0.48 O 7 .

2. The method of claim 1 , wherein combining the nanocrystals with LiNO 3 , LiOH, and Li 2 O 2 comprises combining the nanocrystals with a molten salt flux comprising the LiNO 3 , LiOH, and Li 2 O 2 .

3. The method of claim 2 , wherein the LiNO 3 and the LiOH are present in the molten salt flux in a mass ratio of 1:1.

4. The method of claim 2 , wherein a ratio of the total mass of the LiNO 3 and the LiOH to a total mass of the Li 2 O 2 is about 5:1.

5. The method of claim 1 , comprising heating the mixture to a temperature in a range of 400° C. to 550° C.

6. The method of claim 5 , comprising heating the mixture for a length of time between 1 and 5 hours.

7. The method of claim 1 , further comprising grinding the nanocrystals with the LiNO 3 to yield a precursor mixture.

8. The method of claim 7 , wherein the nanocrystals and the LiNO 3 are present in a mass ratio of about 1:1.

9. A method of synthesizing a tantalum-doped lithium lanthanum zirconate, the method comprising:

combining nanocrystals comprising a tantalum-doped lanthanum zirconate with LiNO 3 , LiOH, and Li 2 O 2 to yield a mixture; and

heating the mixture to yield the tantalum-doped lithium lanthanum zirconate,

wherein combining the nanocrystals with LiNO 3 , LiOH, and Li 2 O 2 comprises combining the nanocrystals with a molten salt flux comprising the LiNO 3 , LiOH, and Li 2 O 2 , and the LiNO 3 and the LiOH are present in the molten salt flux in a mass ratio of 1:1.

10. A method of synthesizing a tantalum-doped lithium lanthanum zirconate, the method comprising:

combining nanocrystals comprising a tantalum-doped lanthanum zirconate with LiNO 3 , LiOH, and Li 2 O 2 to yield a mixture; and

heating the mixture to yield the tantalum-doped lithium lanthanum zirconate,

wherein combining the nanocrystals with LiNO 3 , LiOH, and Li 2 O 2 comprises combining the nanocrystals with a molten salt flux comprising the LiNO 3 , LiOH, and Li 2 O 2 , and a ratio of the total mass of the LiNO 3 and the LiOH to a total mass of the Li 2 O 2 is about 5:1.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 15, 2023
From: WELLER, JON; CHAN, CANDACE
To: ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY
Reel/Frame 064593/0037 →
Continuity (4)
Continuation 17396967 · Aug 9, 2021
Division 16399331 · Apr 30, 2019
Provisional Application 62667383 · May 4, 2018
Related Publication 20230391633A1 · Dec 7, 2023
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