Synthesis of lithium lanthanum zirconate from nanocrystalline lanthanum zirconate

Patent metadata

Field	Value
Publication number	US-12304832-B2
Application number	US-202318449209-A
Country	US
Kind code	B2
Filing date	Aug 14, 2023
Priority date	May 4, 2018
Publication date	May 20, 2025
Grant date	May 20, 2025

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 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.

Assignees

• Weller Jon
• Chan Candace
• Univ Arizona State

Inventors

• Weller Jon
• Chan Candace

Classifications

• C08K5/09

  Carboxylic acids; Metal salts thereof; Anhydrides thereof · CPC title

• C01P2004/04

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

• C01P2002/72

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

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• C01P2002/60

  Compounds characterised by their crystallite size · CPC title