IP Library › Granted Patent US 10,343,131
Granted Patent B1
US 10,343,131 · App. 14/996,914 · Granted Jul 9, 2019

High temperature, hydrophobic, flexible aerogel composite and method of making same

Inventors: Frances I. Hurwitz (Shaker Heights, OH); Haiquan Guo (Avon, OH)
Assignee: The United States of America as Represented by the Administrator of National Aeronautics and Space Administration
B01J13/0091C09K5/00
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Quick Facts
Patent No.
US 10,343,131
App. No.
14/996,914
Granted
Jul 9, 2019
Kind
B1
Abstract

Aerogels, aerogel composites and methods of making the same are discussed. One example method can include the act of creating a Boehmite colloid and adding a hydrolyzed silicon precursor to form a sol. A reinforcement can be infused with the sol, gelled to form a gel, then dried to form an aerogel composite. Such a method can also include the acts of performing one or more solvent exchanges and subjecting the gel composite to supercritical drying. Additionally, such a method can include the act of heat treating the aerogel composite. The aerogel composite can be used in high temperature, flexible seals capable of withstanding temperatures, pressures, and compression levels associated with aerodynamic heating generated during flight and in aerospace applications. The aeorogel composite also can be used in thermal protection systems designed for fire protection for structures or in personnel fire protective equipment.

Claims (21)

1. A method comprising:

creating a sol by:

dispersing an alumina powder in a solution to form a colloid; and

adding a hydrolyzed silicon precursor to the colloid;

infusing one or more reinforcements with the sol and allowing the reinforcement-infused sol to gel at an ambient or heated temperature to form a gel composite;

performing one or more solvent exchanges on the gel composite;

modifying a surface of the gel composite by submersing the gel composite in an organosilane mixture so as to incorporate organosilane groups on the surface of the gel composite; and

subjecting the gel composite to supercritical drying to form an aerogel composite.

2. The method of claim 1 , wherein the solution includes one of water or an aqueous acid solution.

3. The method of claim 1 further comprising heating the aerogel composite to form θ and/or δ alumina and mullite.

4. The method of claim 1 , wherein the addition of silicon is controlled so that the formation of α-alumina can be avoided on heating to 1200° C.

5. The method of claim 1 , wherein the alumina powder is a Boehmite powder such that the aerogel composite contains a Boehmite-derived aerogel having a linear shrinkage that is less than or equal to 5.3%.

6. The method of claim 1 , further comprising controlling cristobalite formation in hydrophobic aerogels and their composites through choice of an organosilane in the organosilane mixture.

7. The method of claim 1 , wherein the aerogel composite is able to maintain a mesoporous structure after heat treatment at 1100° C. for periods of at least 24 hours or at 1200° C. for periods of less than 24 hours.

8. The method of claim 1 , wherein prior to infusing one or more reinforcements with the sol and allowing the reinforcement-infused sol to gel to form a gel composite, the method further comprising coating the one or more reinforcements with a radiation opacifier prior to impregnation of the reinforcement with the precursor sol.

9. The method of claim 8 , wherein the one or more reinforcements includes a ceramic fibrous reinforcement.

10. The method of claim 8 , wherein the radiation opacifier is one of a titania, zirconia, silicon carbide and carbon.

11. The method of claim 8 , wherein the radiation opacifier is capable of absorbing radiation in the infrared region.

12. The method of claim 1 , wherein the alumina powder is a Boehmite powder, further comprising heating the aerogel composite to convert Boehmite to γ and/or η alumina.

13. The method of claim 1 further comprising heating the aerogel composite to form θ and/or δ alumina.

14. The method of claim 1 , wherein the sol is an alumina sol or an aluminosilicate sol, wherein a colloidal or particulate opacifier is dispersed in the alumina or aluminosilicate sol prior to infiltration of the fibrous reinforcement.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 7, 2016
From: HURWITZ, FRANCES I., DR.; GUO, HAIQUAN, MS.
To: US GOVERNMENT ADMINISTRATOR OF NASA
Reel/Frame 039661/0271 →
Continuity (5)
Continuation In Part 14456043 · Aug 11, 2014
Provisional Application 62104206 · Jan 16, 2015
Provisional Application 62236381 · Oct 2, 2015
Provisional Application 61711372 · Aug 16, 2013
Provisional Application 61907662 · Nov 22, 2013