IP Library Granted Patent US 10,391,466
Granted Patent B2
US 10,391,466 · App. 15/612,702 · Granted Aug 27, 2019

Fabrication of nanoporous aerogels via freeze substitution of nanowire suspensions

Inventors: Tyler M. Fears (Pleasanton, CA); Jeffrey D. Colvin (Pleasanton, CA); Sergei O. Kucheyev (Oakland, CA)
Assignee: Lawrence Livermore National Security, LLC
B01J13/0091
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Quick Facts
Patent No.
US 10,391,466
App. No.
15/612,702
Granted
Aug 27, 2019
Kind
B2
Abstract

A method of making a nanoporous aerogel includes the steps of providing nanowire suspensions, freeze casting the nanowire suspensions to produce freeze-cast gels, extracting the frozen medium from the freeze-cast gels by freeze-substitution with a solvent to produce wet gels, modifying or functionalizing the wet gels as needed, and drying the wet gels to produce a nanoporous aerogel.

Claims (26)

1. A method of making a nanoporous aerogel, comprising:

provide a liquid droplet of a nanowire suspension,

provide a cryogenic bath,

freeze cast said nanowire suspension by placing said liquid droplet of a nanowire suspension in said cryogenic bath to produce a spherical freeze-cast gel wherein said spherical freeze-cast gel contains a frozen medium,

provide a container of solvent,

extract said frozen medium from said spherical freeze-cast gel by freeze-substitution by cooling said spherical freeze-cast gel in said container of solvent to produce a spherical wet gel, and

dry said spherical wet gel to produce the nanoporous aerogel.

2. The method of making a nanoporous aerogel of claim 1 wherein said step of drying said spherical wet gel comprises providing a pressure vessel containing a bath of flowing carbon dioxide, placing said spherical wet gel in said bath of flowing carbon dioxide, and venting said carbon dioxide under supercritical conditions.

3. The method of making a nanoporous aerogel of claim 1 wherein said step of providing a liquid droplet of a nanowire suspension comprises providing a liquid droplet of a nanowire suspension comprising a nanowire suspension of carbon nanotubes.

4. The method of making a nanoporous aerogel of claim 1 wherein said step of providing a liquid droplet of a nanowire suspension comprises providing a liquid droplet of a nanowire suspension comprising a nanowire suspension of metal nanowires.

5. The method of making a nanoporous aerogel of claim 1 wherein said step of providing a liquid droplet of a nanowire suspension comprises providing a liquid droplet of a nanowire suspension comprising an aqueous metal nanowire suspension.

6. The method of making a nanoporous aerogel of claim 5 wherein said step of providing a liquid droplet of a nanowire suspension comprising an aqueous metal nanowire suspension comprises providing a liquid droplet of a nanowire suspension comprising an aqueous silver nanowire suspension.

7. The method of making a nanoporous aerogel of claim 1 wherein said step of providing a liquid droplet of a nanowire suspension comprises providing a liquid droplet of a nanowire suspension comprising a non-aqueous metal nanowire suspension.

8. The method of making a nanoporous aerogel of claim 7 wherein said step of providing a non-aqueous metal nanowire suspension comprises providing a non-aqueous gold nanowire suspension.

9. The method of making a nanoporous aerogel of claim 7 wherein said step of providing a non-aqueous metal nanowire suspension comprises providing a non-aqueous copper nanowire suspension.

10. The method of making a nanoporous aerogel of claim 1 wherein said step of freeze casting said nanowire suspension to produce a spherical freeze-cast gel comprises placing said liquid droplet of nanowire suspension in said cryogenic bath comprises placing said liquid droplet of nanowire suspension in a cryogenic liquid to produce a spherical freeze-cast gel.

11. The method of making a nanoporous aerogel of claim 1 wherein said step of freeze casting said nanowire suspension to produce a spherical freeze-cast gel comprises placing said nanowires liquid droplet of nanowire suspension in liquid nitrogen to produce a spherical freeze-cast gel.

12. The method of making a nanoporous aerogel of claim 1 wherein said step of extracting said spherical freeze-cast gel in a solvent to produce a spherical wet gel comprises extracting said spherical freeze-cast gel in acetone below −20° C. to produce a spherical wet gel.

13. A method of making a nanoporous Ag aerogel, comprising:

provide aqueous Ag;

add glycerol and water to said aqueous Ag;

provide a liquid droplet of said aqueous Ag, glycerol, and water to produce an aqueous Ag, glycerol, and water suspension;

provide a cryogenic bath;

freeze cast said aqueous Ag, glycerol, and water suspension to produce a spherical freeze-cast Ag gel by placing said aqueous Ag, glycerol, and water suspension in said cryogenic bath;

extract said water and said glycerol from said spherical freeze-cast Ag gel by freeze substitution with acetone to produce a spherical Ag wet gel and

supercritically dry said spherical Ag wet gel to produce the nanoporous Ag aerogel.

Assignments (3)
CONFIRMATORY LICENSE Recorded Jun 21, 2017
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 042766/0552 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 5, 2017
From: COLVIN, JEFFREY D.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 042594/0356 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 2, 2017
From: FEARS, TYLER M.; KUCHEYEV, SERGEI O.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 042578/0698 →
Continuity (1)
Related Publication 20180345240A1 · Dec 6, 2018