Synthesis of nanosized cubic lithium lanthanum zirconate fast ion conductor

Patent metadata

Field	Value
Publication number	US-11053134-B2
Application number	US-201816111939-A
Country	US
Kind code	B2
Filing date	Aug 24, 2018
Priority date	Aug 25, 2017
Publication date	Jul 6, 2021
Grant date	Jul 6, 2021

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.

First claim

What is claimed is:

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.

Assignees

• Weller Jon Mark
• Chan Candace
• Univ Arizona State

Inventors

• Weller Jon Mark
• Chan Candace

Classifications

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2002/85

  by XPS, EDX or EDAX data · CPC title

• H01M2300/0077

  based on zirconium oxide · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title