IP Library Granted Patent US 8,663,742
Granted Patent B2
US 8,663,742 · App. 13/121,150 · Granted Mar 4, 2014

Durable polymer-aerogel based superhydrophobic coatings, a composite material

Inventors: David J. Kissel (Anoka, MN); Charles Jeffrey Brinker (Albuquerque, NM)
Assignee: STC.UNM
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Quick Facts
Patent No.
US 8,663,742
App. No.
13/121,150
Granted
Mar 4, 2014
Kind
B2
Abstract

Provided are polymer-aerogel composite coatings, devices and articles including polymer-aerogel composite coatings, and methods for preparing the polymer-aerogel composite. The exemplary article can include a surface, wherein the surface includes at least one region and a polymer-aerogel composite coating disposed over the at least one region, wherein the polymer-aerogel composite coating has a water contact angle of at least about 140° and a contact angle hysteresis of less than about 1°. The polymer-aerogel composite coating can include a polymer and an ultra high water content catalyzed polysilicate aerogel, the polysilicate aerogel including a three dimensional network of silica particles having surface functional groups derivatized with a silylating agent and a plurality of pores.

Claims (31)

1. A method for preparing a polymer-aerogel composite coating comprising:

providing a superhydrophobic coating solution, the superhydrophobic coating solution comprising a surface derivatized polysilicate aerogel dispersed in a first solvent, the polysilicate aerogel comprising a three dimensional network of silica particles having surface functional groups derivatized with a silylating agent;

blending a polymer solution and the superhydrophobic coating solution to form a polymer-aerogel solution, wherein the polymer solution comprises one or more polymers dispersed in a second solvent;

dissolving the polymer in the polymer-aerogel blend solution at a first temperature; and

forming, a polymer-aerogel composite coating by applying the polymer-aerogel blend solution to a substrate surface while keeping the polymer-aerogel blend solution at the first temperature, such that the polymer wets the aerogel in the polymer-aerogel composite coating,

wherein the surface derivatized polysilicate aerogel is an ultra high water content acid catalyzed polysilicate aerogel formed using a third solvent, at least one alkoxy silane precursor, water, and an acid, such that a molar ratio of water to alkoxy silane precursor is in the range of about 10 or more, wherein the polysilicate aerogel comprises a three dimensional network of silica particles having surface functional groups and a plurality of pores, and wherein a fluid is disposed in the plurality of pores, the fluid comprising the third solvent; and

prior to blending the polymer solution and the superhydrophobic coating solution, replacing the fluid disposed in the plurality of pores of the polysilicate aerogel with a fourth solvent, wherein the fourth solvent is immiscible with the third solvent.

2. The method for preparing a polymer-aerogel composite coating, according to claim 1 , further comprising:

derivatizing the surface functional groups using a silylating agent to form a surface derivatized polysilicate aerogel; and

forming a superhydrophobic coating solution of the surface derivatized polysilicate aerogel in the first solvent.

3. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the alkoxy silane precursor comprises one or more silane compounds selected from the group consisting of methyltrimethoxy silane, vinyltrimethoxy silane, dimethyldiethoxy silane, methacryloxypropyltrimethoxy silane, mercaptopropyltrimethoxy silane, chloropropyltrimethoxy silane, bromopropyltrimethoxy silane, iodopropyltrimethoxy silane, and chloromethyltrimethoxy silane, tetraethoxysilane, tetramethoxysilane, and 1,2-bis(triethoxysilyl)ethane.

4. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the silylating agent comprises at least one compound selected from the group consisting of trimethylchlorosilane, trichloromethylsilane, trichlorooctylsilane, hexamethyldisilazane and a silane comprising at least one hydrophobic ligand.

5. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the third solvent is the same as the first solvent.

6. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the step of replacing the third solvent present in the plurality of pores of the polysilicate aerogel with the fourth solvent comprises:

(a) breaking up the ultra high water content acid catalyzed polysilicate aerogel to form a broken gel;

(b) adding the fourth solvent to the broken gel at a temperature in the range of about 40° C. to about 60° C. for at least about 30 minutes;

(c) removing a portion of the fourth solvent and the third solvent from the broken gel; and

(d) repeating steps b and c at least three times.

7. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the step of derivatizing the surface functional groups using a silylating agent to form a surface derivatized polysilicate aerogel comprises:

gradually adding to the polysilicate aerogel a silylating agent, the silylating agent comprising at least one compound selected from the group consisting of trimethylchlorosilane, trichloromethylsilane, trichlorooctylsilane, hexamethyldisilazane and a silane comprising at least one hydrophobic ligand;

storing the polysilicate aerogel in silylating agent at a temperature in the range of about 40° C. to about 60° C. for about 6 hours to about 10 hours to form a surface derivatized polysilicate aerogel; and

removing a portion of the silylating agent.

8. The method for preparing a polymer-aerogel composite coating, according to claim 2 , wherein the step of forming a coating solution of the surface derivatized polysilicate aerogel in a first solvent comprises:

washing the surface derivatized polysilicate aerogel with the fourth solvent;

washing the surface derivatized polysilicate aerogel with the first solvent at least twice; and

adding the first solvent to the surface derivatized polysilicate aerogel to form a coating solution.

9. The method for preparing a polymer-aerogel composite coating, according to claim 1 , wherein the first solvent is the same as the second solvent.

10. The method for preparing a polymer-aerogel composite coating, according to claim 1 , wherein the polymer comprises at least one compound selected from the group consisting of poly(methyl methacrylate), polystyrene, poly(butyl methacrylate), poly(tert-butyl methacrylate), poly(methyl acrylate), poly(butyl acrylate), poly(tert-butyl acrylate), poly(perfluorooctyl methacrylate) and a vinyl polymer.

11. The method for preparing a polymer-aerogel composite coating, according to claim 1 , wherein the step of forming a polymer-aerogel composite coating comprises applying the polymer-aerogel blend solution using at least one of dip coating, brush coating, roller coating, spray coating, spin coating, casting, and flow coating.

12. The method for preparing a polymer-aerogel composite coating, according to claim 1 , wherein the step of forming a polymer-aerogel composite coating further comprises heating the substrate to a second temperature greater than the first temperature.

13. The method for preparing a polymer-aerogel composite coating, according to claim 1 , wherein the substrate surface comprises at least one material selected from the group consisting of a metal, silicon, a glass, a ceramic, a plastic and a fabric.

Assignments (4)
CONFIRMATORY LICENSE Recorded Dec 14, 2020
From: NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 054638/0079 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 3, 2018
From: STC.UNM
To: STC.UNM; NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
Reel/Frame 046258/0513 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 30, 2011
From: KISSEL, DAVID J; BRINKER, C. JEFFREY
To: THE REGENTS OF THE UNIVERSITY OF NEW MEXICO C/O RESEARCH & TECHNOLOGY LAW
Reel/Frame 027303/0307 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 30, 2011
From: THE REGENTS OF THE UNIVERSITY OF NEW MEXICO C/O RESEARCH & TECHNOLOGY LAW
To: STC.UNM
Reel/Frame 027303/0563 →
Continuity (2)
Provisional Application 61077143 · Jun 30, 2008
Related Publication 20110206925A1 · Aug 25, 2011