Large scale synthesis of resorcinol-formaldehyde aerogel

Patent metadata

Field	Value
Publication number	US-11535521-B2
Application number	US-202016784385-A
Country	US
Kind code	B2
Filing date	Feb 7, 2020
Priority date	Feb 7, 2020
Publication date	Dec 27, 2022
Grant date	Dec 27, 2022

Abstract

A product includes an aerogel having a single bulk structure, the single bulk structure having at least one dimension greater than 10 millimeters. The single bulk structure includes a plurality of pores, where each pore has a largest diameter defined as a greatest distance between pore walls of the respective pore. In addition, an average of the largest diameters of a majority of the pores is within a specified range, and the plurality of pores are distributed substantially homogenously throughout the single bulk structure.

First claim

What is claimed is:

1. A method of forming a single bulk aerogel having a linear dimension greater than 10 millimeters and having a homogenous distribution of pores throughout, the method comprising:
mixing a solution comprising resorcinol and formaldehyde, wherein the solution has a volume greater than 100 milliliters;
heating the solution to a first temperature for a first defined duration of time;
cooling the solution to a second temperature lower than the first temperature; and
curing the solution for gelation of the solution,
wherein the curing occurs at about the second temperature for a second defined duration of time.

2. The method as recited in claim 1 , wherein the first temperature is in a range of about 40° C. to about 60° C.

3. The method as recited in claim 1 , wherein the first defined duration of time is in a range of greater than 30 minutes to about 6 hours.

4. The method as recited in claim 1 , wherein the volume is greater than 500 milliliters.

5. The method as recited in claim 1 , wherein the solution comprises an additive for tuning a size of a plurality of pores throughout the single bulk aerogel.

6. The method as recited in claim 5 , wherein the additive is selected from the group consisting of: a salt and a surfactant.

7. The method as recited in claim 1 , wherein the curing includes casting the solution into a pre-form having at least one dimension greater than 10 millimeters, wherein the pre-form is selected from the group consisting of: a mold and a template.

8. The method as recited in claim 1 , wherein the second defined duration of time is in a range of greater than 24 hours to about 5 days.

9. The method as recited in claim 1 , further comprising,
machining the single bulk aerogel to have at least one defined characteristic selected from the group consisting of: a size, a shape, and a dimension.

10. The method as recited in claim 9 , wherein the machining includes removing a layer on an outer side of the single bulk aerogel.

11. The method as recited in claim 9 , further comprising, drying the machined single bulk aerogel.

12. The method as recited in claim 11 , wherein the drying is at the second temperature under an air flow.

13. The method as recited in claim 11 , further comprising,
heating the dried single bulk aerogel at a third temperature in an inert gas for carbonizing the single bulk aerogel.

14. The method as recited in claim 13 , further comprising,
activating the carbonized single bulk aerogel at a fourth temperature in a carbon dioxide flow by varying a pressure according to a predefined pattern to create activation in the carbonized single bulk aerogel.

15. The method as recited in claim 14 , wherein a layer of a porous material is proximate to the carbonized single bulk aerogel during the activation of the carbonized single bulk aerogel,
wherein the activation is uniform across the entire carbonized single bulk aerogel.

Assignees

• L Livermore Nat Security Llc

Inventors

• Loeb Colin
• Campbell Patrick
• Knipe Jennifer Marie
• Stadermann Michael

Classifications

• C08J9/286 Primary

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title

• C01B32/336

  characterised by gaseous activating agents · CPC title

• C08J9/36

  After-treatment (C08J9/22 takes precedence) · CPC title

• B29K2105/04

  cellular or porous · CPC title

• B29C39/26

  Moulds or cores · CPC title