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

Patent metadata

Field	Value
Publication number	US-11597658-B2
Application number	US-202017112228-A
Country	US
Kind code	B2
Filing date	Dec 4, 2020
Priority date	Jun 16, 2017
Publication date	Mar 7, 2023
Grant date	Mar 7, 2023

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.

First claim

What is claimed is:

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.

Assignees

• Weller Jon Mark
• Chan Candace
• Univ Arizona State

Inventors

• Weller Jon Mark
• Chan Candace

Classifications

• C01P2002/76

  by a space-group or by other symmetry indications · CPC title

• Y02E60/10

  Energy storage using batteries · 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