Granted Patent
B2
US 12,227,427 · App. 17/366,990 · Granted Feb 18, 2025
Synthesis of nanosized cubic lithium lanthanum zirconate fast ion conductor
C01G25/006H01M10/0525H01M10/0562C01P2002/72C01P2002/74C01P2002/76C01P2002/85C01P2004/04C01P2004/51C01P2004/62C01P2004/64C01P2006/40H01M2300/0077
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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.
Claims (27)
1. A method of synthesizing tantalum-doped lithium lanthanum zirconate, the method comprising:
combining a reagent composition with a molten salt composition to yield a salt reaction medium, wherein the reagent composition comprises a lithium component, a lanthanum component, a zirconium component, and a tantalum component;
heating the salt reaction medium to a temperature in a range of 500° C. to 1000° C. to yield a reaction product comprising tantalum-doped 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,
lithium hydroxide,
a eutectic mixture of lithium chloride and lithium hydroxide,
a eutectic mixture of lithium bromide and potassium bromide, and
a eutectic mixture of sodium chloride and potassium chloride.
2. The method of claim 1 , wherein the lithium component comprises one or both of lithium nitrate and lithium hypochlorite.
3. The method of claim 1 , wherein the lanthanum component comprises one or both of lanthanum nitrate and lanthanum oxychloride.
4. The method of claim 1 , wherein the zirconium component comprises zirconium oxynitrate.
5. The method of claim 1 , wherein the tantalum component comprises tantalum pentoxide.
6. The method of claim 1 , wherein the salt reaction medium comprises an extrinsic dopant.
7. The method of claim 6 , wherein the extrinsic dopant comprises a gallium component.
8. The method of claim 7 , wherein a molar ratio of the lithium component, the lanthanum component, the zirconium component, the tantalum component, and the gallium component in the reagent composition is 7:3:1.4:0.6:0.25.
9. The method of claim 1 , wherein the salt composition is a eutectic mixture of potassium chloride and lithium chloride, and a weight ratio of the reagent composition to the salt composition in the salt reaction medium is 1:3.
10. The method of claim 9 , wherein the salt reaction medium further comprises sodium fluoride up to 25% by mass.
11. The method of claim 1 , wherein the salt composition is lithium hydroxide, and a weight ratio of the reagent composition to the salt composition in the salt reaction medium is 1:2.
12. The method of claim 1 , wherein the salt composition is a eutectic mixture of lithium bromide and potassium bromide, and a weight ratio of the reagent composition to the salt composition in the salt reaction medium is 1:1.
13. The method of claim 1 , wherein the salt composition is a eutectic mixture of sodium chloride and potassium chloride, and a weight ratio of the reagent composition to the salt composition in the salt reaction medium is 1:1.
14. 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.
15. The method of claim 1 , wherein heating the salt reaction medium comprises heating to a temperature in a range of 550° C. to 900° C.
16. The method of claim 1 , wherein the tantalum-doped lithium lanthanum zirconate is represented by Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 .
17. The method of claim 16 , wherein the components of the reagent composition are present in the salt reaction medium in stoichiometric proportions.
18. The method of claim 1 , wherein the tantalum-doped lithium lanthanum zirconate is in the form of nanoparticles.
19. The method of claim 18 , wherein a maximum dimension of the nanoparticles is between 300 nm and 500 nm.
Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST
Recorded Sep 20, 2021
From: WELLER, JON MARK; CHAN, CANDACE
To: ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY
Reel/Frame 057532/0819 →
Continuity (3)
Provisional Application
62550155
· Aug 25, 2017
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