IP Library › Granted Patent US 10,633,256
Granted Patent B1
US 10,633,256 · App. 15/491,168 · Granted Apr 28, 2020

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

Inventors: Haiquan Guo (Avon, OH); Frances I. Hurwitz (Shaker Heights, OH)
Assignee: United States of America as Represented by the Administrator of National Aeronautics and Space Administration
C01B33/157F16L59/028
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Quick Facts
Patent No.
US 10,633,256
App. No.
15/491,168
Granted
Apr 28, 2020
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 subcritical 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 aerogel composite also can be used in thermal protection systems designed for fire protection for structures or in personnel fire protective equipment.

Claims (35)

1. A method comprising:

creating a sol by dispersion of an alumina powder in a solvent to form a colloid and adding a hydrolyzed silicon precursor to the colloid;

adding an opacifier to the sol;

infusing a reinforcement with the sol;

allowing the infused sol to gel from an acid solution to form a gel composite;

submersing the gel composite in a organosilane or organosilane/solvent mixture so as to incorporate organosilane groups on a surface of the gel composite; and

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

2. The method of claim 1 , wherein after submersing the gel composite in the organosilane or organosilane/solvent mixture, the method further comprises transferring the gel composite to a non-polar solvent.

3. The method of claim 2 , wherein the non-polar solvent is selected from the group consisting of hexane, heptane, pentane, cyclohexane, octane, dimethyl ether, chloroform, dichloromethane, dimethyl formamide, or a combination of two or more thereof.

4. The method of claim 3 , wherein the non-polar solvent is hexane.

5. The method of claim 1 , wherein the gel composite is dried in a vacuum oven at 10 −2 -10 −3 atm.

6. A method comprising:

creating a sol by dispersion of an alumina powder in a solvent 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 from an acid solution to form a gel composite,

coating the one or more reinforcements with an opacifier prior to infusing the one or more reinforcements with the sol;

performing one or more solvent exchanges on the gel composite;

submersing the gel composite in a organosilane or organosilane/solvent mixture so as to incorporate organosilane groups on a surface of the gel composite; and

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

7. The method of claim 6 , wherein the one or more reinforcements includes a ceramic fibrous reinforcement.

8. The method of claim 6 , wherein prior to infusing one or more reinforcements with the sol and allowing the reinforcement-infused sol to gel from an acid solution to form a gel composite, the method further comprising applying a coating the one or more reinforcements which acts as a radiation opacifier prior to impregnation of the reinforcement with the precursor sol.

9. The method of claim 8 , wherein the coating is one of a titania, zirconia, silicon carbide, carbon, or a combination of two or more thereof.

10. A method, comprising:

creating an alumina colloid;

adding a hydrolyzed silicon precursor to the colloid to create a sol;

infusing one or more reinforcements with the sol and allowing the reinforcement-infused sol to gel from an acid solution to form a gel composite;

coating the one or more reinforcements with an opacifier prior to infusing the one or more reinforcements with the sol;

performing one or more solvent exchanges on the gel composite;

subjecting the gel composite to subcritical drying to form an aerogel composite; and

heat treating the aerogel composite.

11. The method of claim 10 , wherein after the one or more solvent exchanges, the method further comprises transferring the gel composite to a non-polar solvent.

12. The method of claim 11 , wherein the non-polar solvent is hexane.

13. The method of claim 10 , wherein the gel composite is dried in a vacuum oven at 10 −2 -10 −3 atm.

14. The method of claim 10 , wherein the alumina comprises boehmite and the hydrolyzed silicon precursor comprises tetraethyl orthosilicate (TEOS) hydrolyzed in a solution.

15. The method of claim 10 , comprising adding an opacifier to the hydrolyzed silicon precursor prior to adding the precursor to the colloid.

16. The method of claim 15 , wherein the opacifier comprises at least one of titanium dioxide, zirconium dioxide, or silicon carbide.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 19, 2017
From: GUO, HAIQUAN, MS.; HURWITZ, FRANCES I., MS.
To: US GOVT ADMINISTRATOR OF NASA
Reel/Frame 042067/0969 →
Continuity (4)
Continuation In Part 14996914 · Jan 15, 2016
Continuation In Part 14456043 · Aug 11, 2014
Provisional Application 62324585 · Apr 19, 2016
Provisional Application 62236381 · Oct 2, 2015
Cited By (4)
US 12,503,400 US 12,509,399 US 12,534,409 US 12,552,674