IP Library Granted Patent US 10,336,937
Granted Patent B2
US 10,336,937 · App. 15/073,400 · Granted Jul 2, 2019

Monolithic rare earth oxide aerogels

Inventors: Marcus A. Worsley (Hayward, CA); Alexander E. Gash (Brentwood, CA); Robert A. Reibold (Salida, CA)
Assignee: Lawrence Livermore National Security, LLC
C09K11/7701C01F17/0018C01F17/0043C04B38/009C01P2002/85C01P2004/03C01P2004/04C01P2006/10C01P2006/12C01P2006/14C01P2006/16C01P2006/60C01P2006/80
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Quick Facts
Patent No.
US 10,336,937
App. No.
15/073,400
Granted
Jul 2, 2019
Kind
B2
Abstract

Disclosed here is a method for making a monolithic rare earth oxide (REO) aerogel, comprising: preparing a reaction mixture comprising at least one rare earth metal nitrate, at least one epoxide, at least one base catalyst, and at least one organic solvent; curing the mixture to produce a wet gel; drying the wet gel to produce a dry gel; and thermally annealing the dry gel to produce the monolithic REO aerogel. Also disclosed is an REO aerogel comprising a network of REO nanostructures, wherein the REO aerogel is a monolith having at least one lateral dimension of at least 1 cm, wherein the REO aerogel has a density of about 40-500 mg/cm 3 and/or a BET surface area of at least about 20 m 2 /g, and wherein the REO aerogel is substantially free of oxychloride.

Claims (15)

1. A method for making a monolithic rare earth oxide (REO) aerogel, comprising:

preparing a reaction mixture consisting essentially of at least one rare earth metal nitrate, at least one epoxide, at least one base catalyst, and at least one organic solvent, wherein the reaction mixture is substantially free of chloride;

curing the mixture to produce a wet gel;

drying the wet gel to produce a dry gel; and

thermally annealing the dry gel to produce the monolithic REO aerogel.

2. The method of claim 1 , wherein the reaction mixture comprises at least two different rare earth metal nitrates.

3. The method of claim 1 , wherein the at least one base catalyst is selected from the group consisting of ammonium carbonate, sodium carbonate, sodium hydroxide, ammonium hydroxide, and ammonia vapor.

4. The method of claim 1 , wherein the at least one base catalyst comprises ammonium carbonate.

5. The method of claim 1 , wherein the at least one epoxide comprises propylene oxide.

6. The method of claim 1 , wherein the at least one organic solvent comprises alcohol.

7. The method of claim 1 , wherein the reaction mixture is cured at a temperature of about 50°-100° C.

8. The method of claim 1 , wherein the drying step comprises washing in acetone or dry alcohol.

9. The method of claim 1 , wherein the drying step comprises supercritical drying or ambient drying.

10. The method of claim 1 , wherein the dry gel is thermally annealed in air or in an inert atmosphere at a temperature of about 500° C. or higher.

11. The method of claim 1 , wherein the REO aerogel is produced in less than about 120 hours starting from the curing step to completion of the thermal annealing step.

Assignments (3)
CONFIRMATORY LICENSE Recorded May 18, 2016
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 038630/0160 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 21, 2016
From: WORSLEY, MARCUS A.; REIBOLD, ROBERT A.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 038048/0226 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 21, 2016
From: GASH, ALEXANDER A.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 038048/0247 →
Continuity (1)
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