Monolithic rare earth oxide aerogels

Patent metadata

Field	Value
Publication number	US-10336937-B2
Application number	US-201615073400-A
Country	US
Kind code	B2
Filing date	Mar 17, 2016
Priority date	Mar 17, 2016
Publication date	Jul 2, 2019
Grant date	Jul 2, 2019

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/cm3 and/or a BET surface area of at least about 20 m2/g, and wherein the REO aerogel is substantially free of oxychloride.

First claim

What is claimed is:

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.

Assignees

• L Livermore Nat Security Llc

Inventors

• Worsley Marcus A
• Gash Alexander E
• Reibold Robert A

Classifications

• C01F17/32

  oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO · CPC title

• C04B38/009

  Porous or hollow ceramic granular materials, e.g. microballoons (C04B18/027, C04B20/002 take precedence) · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C01P2006/60

  Optical properties, e.g. expressed in CIELAB-values · CPC title

• C01P2006/10

  Solid density · CPC title