IP Library Granted Patent US 9,963,394
Granted Patent B2
US 9,963,394 · App. 15/010,875 · Granted May 8, 2018

Method for producing dense lithium lanthanum tantalate lithium-ion conducting ceramics

Inventors: Harlan James Brown-Shaklee (Albuquerque, NM); Jon Ihlefeld (Albuquerque, NM); Erik David Spoerke (Albuquerque, NM); Mia Angelica Blea-Kirby (Albuquerque, NM)
Assignee: National Technology & Engineering Solutions of Sandia, LLC
C04B35/495C04B35/6261C04B35/62645C04B35/64C04B2235/3203C04B2235/3227C04B2235/443C04B2235/449C04B2235/5436C04B2235/6567C04B2235/668C04B2235/77C04B2235/80C04B2235/81
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Quick Facts
Patent No.
US 9,963,394
App. No.
15/010,875
Granted
May 8, 2018
Kind
B2
Abstract

A method to produce high density, uniform lithium lanthanum tantalate lithium-ion conducting ceramics uses small particles that are sintered in a pressureless crucible that limits loss of Li 2 O.

Claims (18)

1. A method for producing a lithium lanthanum tantalate ceramic, comprising:

dissolving lithium nitrate in an alcohol solvent;

dissolving lanthanum acetate in an acid solvent;

suspending tantalum oxide in an alcohol;

blending the lithium nitrate solution, the lanthanum acetate solution, and the tantalum oxide suspension and evaporating the solvents to provide a stoichiometric mixture;

combusting the stoichiometric mixture at a sufficiently high temperature to remove organics, thereby providing an inorganic mixture;

calcining the inorganic mixture at a sufficiently high temperature to remove carbonates, thereby providing a mixed oxide powder; and

sintering the mixed oxide powder in a closed and non-reactive crucible at a sufficiently high temperature and pressure to provide a dense lithium lanthanum tantalate ceramic.

2. The method of claim 1 , wherein the alcohol solvent for dissolving lithium nitrate comprises ethanol.

3. The method of claim 1 , wherein the acid solvent for dissolving lanthanum acetate comprises propionic acid.

4. The method of claim 1 , wherein the alcohol for suspending tantalum oxide comprises ethanol.

5. The method of claim 1 , wherein the sufficiently high temperature for combusting is greater than 500° C.

6. The method of claim 1 , wherein the sufficiently high temperature for calcining is greater than 800° C.

7. The method of claim 1 , wherein the sufficiently high temperature for sintering is greater than 1000° C.

8. The method of claim 1 , wherein the sufficiently high pressure for sintering is ambient pressure.

9. The method of claim 1 , wherein the closed and non-reactive crucible comprises a platinum crucible.

10. The method of claim 1 , wherein the closed and non-reactive crucible comprises a transition metal crucible.

11. The method of claim 10 , wherein the transition metal comprises nickel, platinum, palladium, iridium, or alloys thereof.

Assignments (3)
CHANGE OF NAME Recorded Apr 2, 2018
From: SANDIA CORPORATION
To: NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
Reel/Frame 046419/0517 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 4, 2016
From: BROWN-SHAKLEE, HARLAN JAMES; IHLEFELD, JON; SPOERKE, ERIK DAVID; BLEA-KIRBY, MIA ANGELICA
To: SANDIA CORPORATION
Reel/Frame 039932/0950 →
CONFIRMATORY LICENSE Recorded Apr 11, 2016
From: SANDIA CORPORATION
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 038241/0255 →
Continuity (2)
Provisional Application 62110834 · Feb 2, 2015
Related Publication 20160221880A1 · Aug 4, 2016