Large scale synthesis of resorcinol-formaldehyde aerogel

Patent metadata

Field	Value
Publication number	US-2021246032-A1
Application number	US-202016784385-A
Country	US
Kind code	A1
Filing date	Feb 7, 2020
Priority date	Feb 7, 2020
Publication date	Aug 12, 2021
Grant date	—

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

2 . The product as recited in claim 1 , wherein an average of the largest diameters of a majority of the pores is in a range of about 500 nanometers to about 2000 nanometers.

3 . The product as recited in claim 1 , wherein an average of the largest diameters of a majority of the pores is in a range of greater than 50 nanometers to about 500 nanometers.

4 . The product as recited in claim 1 , wherein an average of the largest diameters of a majority of the pores is in a range of about 2 microns to about 10 microns.

5 . The product as recited in claim 1 , wherein an average of the largest diameters of a majority of the pores is in a range of about 10 microns to about 30 microns.

6 . The product as recited in claim 1 , wherein the single bulk structure has at least one dimension greater than 50 millimeters.

7 . 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.

8 . The method as recited in claim 7 , wherein the first temperature is in a range of about 40° C. to about 60° C.

9 . The method as recited in claim 7 , wherein the first defined duration of time is in a range of greater than 30 minutes to about 6 hours.

10 . The method as recited in claim 7 , wherein the volume is greater than 500 milliliters.

11 . The method as recited in claim 7 , wherein the solution comprises an additive for tuning a size of a plurality of pores throughout the single bulk aerogel.

12 . The method as recited in claim 11 , wherein the additive is selected from the group consisting of: a salt and a surfactant.

13 . The method as recited in claim 7 , 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.

14 . The method as recited in claim 7 , wherein the second defined duration of time is in a range of greater than 24 hours to about 5 days.

15 . The method as recited in claim 7 , 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.

16 . The method as recited in claim 15 , wherein the machining includes removing a layer on an outer side of the single bulk aerogel.

17 . The method as recited in claim 15 , further comprising,
drying the machined single bulk aerogel.

18 . The method as recited in claim 17 , wherein the drying is at the second temperature under an air flow.

19 . The method as recited in claim 17 , further comprising,
heating the dried single bulk aerogel at a third temperature in an inert gas for carbonizing the single bulk aerogel.

20 . The method as recited in claim 19 , 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.

21 . The method as recited in claim 20 , 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

• C04B38/0032

  one of the precursor materials being a monolithic element having approximately the same dimensions as the final article, e.g. a paper sheet which after carbonisation will react with silicon to form a porous silicon carbide porous body · CPC title

• C04B2111/52

  Sound-insulating materials · CPC title

• C04B2111/28

  Fire resistance, i.e. materials resistant to accidental fires or high temperatures · CPC title

• C08G8/22

  Resorcinol · CPC title

• B29K2105/04

  cellular or porous · CPC title