Synthesis of lithium lanthanum zirconate from nanocrystalline lanthanum zirconate

Patent metadata

Field	Value
Publication number	US-11760652-B2
Application number	US-202117396967-A
Country	US
Kind code	B2
Filing date	Aug 9, 2021
Priority date	May 4, 2018
Publication date	Sep 19, 2023
Grant date	Sep 19, 2023

Abstract

Fabricating a layer including lithium lanthanum zirconate (Li7La3Zr2O12) layer includes forming a slurry including lanthanum zirconate (La2Zr2O7) 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.

First claim

What is claimed is:

1. A method of synthesizing lithium lanthanum zirconate Li 7 La 3 Zr 2 O 12 , the method comprising:
combining lanthanum zirconate La 2 Zr 2 O 7 nanocrystals comprising excess lanthanum with LiNO 3 to yield a first mixture;
combining the first mixture with one or more salts of lithium to yield a second mixture;
calcining the second mixture to yield a calcined mixture; and
sintering the calcined mixture to yield the lithium lanthanum zirconate.

2. The method of claim 1 , wherein the lanthanum zirconate nanocrystals further comprise a dopant.

3. The method of claim 1 , wherein the one or more salts of lithium are molten.

4. The method of claim 3 , wherein the one or more salts of lithium consist of LiNO 3 and LiOH.

5. The method of claim 4 , wherein a mass ratio of LiNO 3 to LiOH is about 1:1.

6. The method of claim 3 , wherein the one or more salts of lithium comprise a molten salt flux.

7. The method of claim 6 , wherein the molten salt flux further comprises Li 2 O 2 .

8. The method of claim 6 , wherein a temperature of the molten salt flux is between 400° C. and 550° C.

9. The method of claim 8 , wherein the lanthanum zirconate and the one or more salts of lithium react in the molten salt flux for a length of time between 1 hour and 5 hours to yield the mixture.

10. The method of claim 1 , wherein the mixture is a slurry.

Assignees

• Weller Jon
• Chan Candace
• Univ Arizona State

Inventors

• Weller Jon
• Chan Candace

Classifications

• C09D133/02 Primary

  Homopolymers or copolymers of acids; Metal or ammonium salts thereof · CPC title

• C01G25/006 Primary

  Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/03

  obtained by SEM · CPC title