Synthesis of lithium lanthanum zirconate from nanocrystalline lanthanum zirconate

Patent metadata

Field	Value
Publication number	US-11084734-B2
Application number	US-201916399331-A
Country	US
Kind code	B2
Filing date	Apr 30, 2019
Priority date	May 4, 2018
Publication date	Aug 10, 2021
Grant date	Aug 10, 2021

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 fabricating a layer comprising lithium lanthanum zirconate Li 7 La 3 Zr 2 O 12 the method comprising:
forming a slurry comprising lanthanum zirconate La 2 Zr 2 O 7 nanocrystals, a lithium-containing compound, and a lanthanum-containing compound to yield a dispersion comprising lithium, lanthanum, and zirconium;
dispensing the slurry onto a substrate;
drying the slurry to form a dried slurry; and
calcining the dried slurry to yield the layer comprising lithium lanthanum zirconate.

2. The method of claim 1 , wherein the lithium-containing compound comprises lithium nitrate.

3. The method of claim 1 , wherein the lanthanum-containing compound comprises lanthanum nitrate.

4. The method of claim 1 , wherein the slurry further comprises a dopant.

5. The method of claim 4 , wherein the dopant comprises at least one of aluminum, gallium, tantalum, niobium, and molybdenum.

6. The method of claim 1 , wherein the slurry further comprises a dispersant.

7. The method of claim 6 , wherein the dispersant comprises at least one of a surfactant, fish oil, poly(acrylic acid) and salts thereof, poly(methacrylic acid) and salts thereof, and phosphate esters.

8. The method of claim 1 , wherein the slurry further comprises a plasticizer.

9. The method of claim 8 , wherein the plasticizer comprises polyethylene glycol, benzyl butyl phthalate, glycerol, or a combination thereof.

10. The method of claim 1 , wherein the slurry further comprises a binder.

11. The method of claim 10 , wherein the binder comprises polyvinylbutyral.

12. The method of claim 1 , wherein disposing the slurry on the substrate comprises casting the slurry on the substrate.

13. The method of claim 12 , wherein casting the slurry on the substrate comprises tape-casting or spin-casting.

14. The method of claim 1 , wherein disposing the slurry on the substrate comprises dip-coating the substrate in the slurry.

15. The method of claim 1 , wherein calcining the dried slurry comprises heating the dried slurry at a temperature between 700° C. and 1200° C. for a few minutes to several hours.

16. The method of claim 1 , wherein forming the slurry comprises forming the slurry in methanol, ethanol, or a combination thereof.

17. The method of claim 1 , wherein the lanthanum zirconate nanocrystals have an average diameter in a range of 5 nm to 50 nm.

18. The method of claim 1 , wherein the lanthanum zirconate nanocrystals have an average diameter in a range of 10 nm to 30 nm.

19. The method of claim 1 , wherein the layer comprises lithium lanthanum zirconate having a grain size of less than 300 nm.

20. The method of claim 1 , wherein a thickness of the layer is in a range of 1 μm to 500 μm.

21. The method of claim 1 , wherein the lithium lanthanum zirconate is cubic phase lithium lanthanum zirconate.

22. The method of claim 1 , wherein the dispersion comprises lithium, lanthanum, and zirconium in a molar ratio of 7:3:2.

23. The method of claim 1 , wherein the dispersion comprises lanthanum and zirconium in a molar ratio of >7 moles lithium to 3 moles lanthanum to 2 moles zirconium.

Assignees

• Weller Jon
• Chan Candace
• Univ Arizona State

Inventors

• Weller Jon
• Chan Candace

Classifications

• C01G25/006 Primary

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

• C08K5/053

  Polyhydroxylic alcohols · CPC title

• C01P2002/72

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

• C08K5/09

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

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title