# US 11,078,346 B2 · Systems and methods for producing aerogel materials > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,078,346 B2 - Document ID: US11078346B2 - Status: Granted - Kind: B2 - Application number: 16/724,811 - Filed: 2019-12-23 - Published: 2020-12-03 - Granted: 2021-08-03 - Earliest claimed: 2015-02-05 - Assignees: Aerogel Technologies, LLC - Applicants: Aerogel Technologies, LLC - Inventors: Stephen A. Steiner, III; Justin S. Griffin; Benjamin H. Wunsch; John N. Schneider - Web page: https://patentgrep.com/patent/US11078346B2 ## CPC - C08J 9/28: by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum - C08J 2201/048: Elimination of a frozen liquid phase - C08J 2201/0422: containing oxygen atoms, e.g. saccharose - C08J 2201/0482: the liquid phase being organic - C08J 2205/026: Aerogel, i.e. a supercritically dried gel - C08J 2205/042: Nanopores, i.e. the average diameter being smaller than 0,1 micrometer - C08J 2205/044: Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter - C08J 2361/00: Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers - C08J 2375/00: Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers - C08J 2375/02: Polyureas - C08J 2375/04: Polyurethanes - C08J 2377/00: Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers - C08J 2379/08: Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors - C08J 2383/04: Polysiloxanes - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) ## Abstract Systems and methods for producing aerogel materials are generally described. In certain cases, the methods do not require supercritical drying as part of the manufacturing process. In some cases, certain combinations of materials, solvents, and/or processing steps may be synergistically employed so as to enable manufacture of large (e.g., meter-scale), substantially crack free, and/or mechanically strong aerogel materials. ## Claims ### Claim 1 A method of manufacturing an aerogel, comprising: freezing a solvent within a precursor gel material comprising the solvent; and sublimating the solvent at about atmospheric pressure to produce the aerogel; wherein: the solvent comprises tert-butanol, the aerogel has at least one dimension greater than or equal to about 1 m, the aerogel exhibits a compressive modulus greater than or equal to about 100 kPa, the aerogel exhibits a compressive yield strength greater than or equal to about 20 kPa, and the aerogel has at least one dimension having a length that is within about 20% of the length of a corresponding dimension of the precursor gel material of the aerogel immediately prior to the sublimating. ### Claim 2 (depends on 1) The method of claim 1, wherein the aerogel comprises a polyimide, a polyurea, and/or a polymer-crosslinked oxide. ### Claim 3 (depends on 1) The method of claim 1, wherein the aerogel is reinforced with a fiber. ### Claim 4 (depends on 1) The method of claim 1, wherein the aerogel is reinforced with a fibrous batting. ### Claim 5 (depends on 1) The method of claim 1, wherein the aerogel comprises mesopores. ### Claim 6 (depends on 1) The method of claim 1, wherein at least about 50% of the solvent originally contained within the precursor gel material is recovered. ### Claim 7 (depends on 6) The method of claim 6, wherein the recovered solvent is used to prepare a second aerogel. ### Claim 8 (depends on 1) The method of claim 1, wherein the aerogel exhibits a compressive ultimate strength of greater than 1 MPa. ### Claim 9 (depends on 1) The method of claim 1, wherein the aerogel has a second dimension corresponding to a thickness of greater than 1 mm. ### Claim 10 (depends on 1) The method of claim 1, wherein the aerogel has a bulk density of between about 0.05 g/cc and about 0.3 g/cc. ### Claim 11 (depends on 1) The method of claim 1, wherein the aerogel has a compressive modulus of greater than about 1 MPa. ### Claim 12 (depends on 1) The method of claim 1, wherein the aerogel has a compressive modulus of greater than about 10 MPa. ### Claim 13 (depends on 1) The method of claim 1, wherein the aerogel has a compressive yield strength of greater than about 1 MPa. ### Claim 14 (depends on 1) The method of claim 1, wherein sublimating the solvent comprises providing a flow of gas. ### Claim 15 (depends on 14) The method of claim 14, wherein the temperature of the flowing gas is within about 50° C. of the melting temperature of the solvent. ### Claim 16 (depends on 1) The method of claim 1, wherein the aerogel is substantially crack-free. ### Claim 17 (depends on 1) The method of claim 1, wherein the aerogel is monolithic. ### Claim 18 (depends on 1) The method of claim 1, wherein the solvent has less than about 1.5 v/v % impurities. ### Claim 19 (depends on 1) The method of claim 1, wherein the aerogel has at least one dimension greater than or equal to about 5 m.