IP Library Granted Patent US 9,971,065
Granted Patent B2
US 9,971,065 · App. 13/826,288 · Granted May 15, 2018

Anti-reflection glass made from sol made by blending tri-alkoxysilane and tetra-alkoxysilane inclusive sols

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Quick Facts
Patent No.
US 9,971,065
App. No.
13/826,288
Granted
May 15, 2018
Kind
B2
Abstract

Anti-reflection (AR) coating for a glass substrate is prepared by blending at least two different sols to form a coating sol which is used to coat a substrate such as a transparent glass substrate. In certain example embodiments, a method includes forming a first sol formulation including a colloidal solution having a tri-alkoxysilane based binder; forming a second sol formulation including a colloidal solution having a tetra-alkoxysilane based binder; blending the first and second sol formulations to form a coating sol formulation; coating at least a portion of said coating sol formulation onto the glass substrate to form a coating; and heating (e.g., for curing and/or annealing) the glass substrate and the coating thereon. Anti-reflection glasses show improved mechanical strength and higher transmittances (e.g., Tqe % gain).

Claims (53)

1. A method of making a coated article including an anti-reflection coating on a glass substrate, the method comprising:

forming a first sol formulation comprising a colloidal solution including a tri-alkoxysilane based binder and silica based nanoparticles;

forming a second sol formulation comprising a colloidal solution including a tetra-alkoxysilane based binder and silica based nanoparticles, wherein the second sol formulation comprises a greater percentage by weight of silica nanoparticles than the first sol formulation;

blending the first sol formulation and the second sol formulation to form a coating sol formulation, the first sol formulation and/or the second sol formulation being aged for more than one day prior to said blending;

coating at least a portion of said coating sol formulation onto the glass substrate to form a coating; and

heating said glass substrate and said coating,

wherein visible transmittance is increased by at least 2.8% as a result of said coating being applied on the glass substrate, and

wherein said coating has a refractive index, following said heating, of from about 1.2 to 1.3.

2. A method according to claim 1 , comprising curing the coating via at least said heating.

3. A method according to claim 1 , wherein the tri-alkoxysilane-based binder in the first sol formulation comprises the formula:

wherein R 1 , R 2 , and R 3 are the same or different and each represents an alkyl group containing 1 to 20 carbon atoms, an aryl group containing 6 to 20 carbon atoms, or an aralkyl group containing 7 to 20 carbon atoms; and

wherein R 4 represents an alkyl group containing 1 to 20 carbon atoms, an aryl group containing 6 to 20 carbon atoms, an aralkyl group containing 7 to 20 carbon atoms, or a fluoro-modified alkyl group containing 1 to 20 carbon atoms.

4. A method according to claim 1 , wherein a mass ratio of the tri-alkoxysilane-based binder to the silica based nanoparticles in the first sol formulation is between 0.1:1 to 20:1.

5. The method of claim 1 , wherein the tri-alkoxysilane-based binder comprises from about 10 wt. % to about 80 wt. % ash contribution in the total ash content of the first sol-formulation.

6. The method of claim 1 , wherein the tri-alkoxysilane-based binder is selected from the group consisting of n-propyltriethoxysilane, n-pentyltriethoxysilane, n-hexyltriethoxysilane, cyclohexyltrimethoxysilane, and combinations thereof.

7. The method of claim 1 , wherein the tri-alkoxysilane-based binder comprises cyclohexyltrimethoxysilane.

8. The method of claim 1 , comprising forming a gel on the glass substrate by drying the coating sol formulation coated on the glass substrate prior to heating the coated glass substrate.

9. The method of claim 1 , wherein silica based nanoparticles in each of the first sol formulation, second sol formulation, and coating sol formulation have a shape selected from spherical, elongated, disc-shaped, and combinations thereof.

10. The method of claim 1 , wherein silica based nanoparticles in each of the first sol formulation, second sol formulation, and coating sol formulation are selected from spherical particles having a particle size from about 40 to 50 nm, spherical particles having a particle size from about 70 to 100 nm, spherical particles having a particle size from about 10 to 15 nm, spherical particles having a particle size from about 17 to 23 nm, elongated particles having a diameter from 9 to 15 nm and length of 40 to 100 nm, and combinations thereof.

11. The method of claim 1 , wherein the first sol formulation further comprises an alcohol containing solvent, and an acid or base containing catalyst.

12. A method according to claim 1 , wherein the amount of tetra-alkoxysilane in the second sol formulation is at least 20% by weight of said second sol formulation.

13. A method according to claim 1 , wherein the amount of tetra-alkoxysilane in the coating sol formulation is at least 20% by weight of said coating sol formulation.

14. A method according to claim 1 , wherein said glass substrate is a matte-matte glass.

15. A method according to claim 1 , wherein said glass substrate comprises soda-lime-silica based float glass.

16. A method according to claim 1 , wherein said coating step comprises spin coating or dip coating.

17. A method according to claim 1 , wherein the thickness of said coating after curing is from about 120 to 140 nm.

18. A method according to claim 1 , wherein said heating comprising heating the coated glass substrate at temperature(s) of at least 580 degrees C. for a period of at least about 1 minute.

19. The method of claim 1 , wherein each of said first, second, and coating sol formulations further include water, acetic acid and n-propyl alcohol.

20. The method of claim 1 , wherein said blending comprises providing more of the second sol formulation than the first sol formulation in the coating sol formulation.

21. The method of claim 1 , wherein said coating sol formulation comprises by weight from about 60-80% of the second sol formulation and from about 20-40% of the first sol formulation.

22. The method of claim 1 , wherein the second sol formulation contains at least about 4 wt. % or more silica based nanoparticles than the first sol formulation.

23. The method of claim 1 , wherein the tetra-alkoxysilane based binder of the second sol formulation comprises TEOS.

24. The method of claim 1 , wherein the second sol formulation further comprises an alcohol containing solvent, and an acid or base containing catalyst.

25. The method of claim 1 , wherein the coating is applied directly on the glass substrate.

26. The method of claim 1 , wherein the first sol and/or second sol formulation(s) is/are aged for more than one day and less than or equal to thirty days before said blending.

27. A method of making a coated article including an anti-reflection coating on a glass substrate, the method comprising:

blending together a first sol formulation and a second sol formulation to form a coating sol formulation,

the first sol formulation and/or the second sol formulation each being aged for more than one day prior to said blending,

the first sol formulation comprising a colloidal solution including a tri-alkoxysilane based binder and silica based nanoparticles and

the second sol formulation comprising a colloidal solution including a tetra-alkoxysilane based binder and silica based nanoparticles,

wherein the second sol formulation comprises a greater percentage by weight of silica based nanoparticle than the first sol formulation;

applying at least a portion of said coating sol formulation onto the glass substrate to form an intermediate coating; and

heating said glass substrate and said intermediate coating in forming the anti-reflection coating.

28. The method of claim 27 ,

wherein visible transmittance is increased by at least 3% as a result of said coating being applied on the glass substrate, and

wherein said coating has a refractive index, following said heating, of from about 1.21 to 1.27.

29. A method of making a coated article including an anti-reflection coating on a glass substrate, the method comprising:

forming a first sol formulation comprising a colloidal solution including a tri-alkoxysilane based binder and silica based nanoparticles;

forming a second sol formulation comprising a colloidal solution including a tetra-alkoxysilane based binder and silica based nanoparticles, wherein the second sol formulation comprises a greater per by weight of silica based nanoparticles than the first sol formulation;

blending the first sol formulation and the second sol formulation to form a coating sol formulation;

coating at least a portion of said coating sol formulation onto the glass substrate to form a coating; and

heating said glass substrate and said coating,

wherein visible transmittance is increased by at least 2.8% as a result of said coating being applied on the glass substrate.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 29, 2017
From: GUARDIAN INDUSTRIES CORP.
To: GUARDIAN GLASS, LLC.
Reel/Frame 044053/0318 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 26, 2017
From: GUARDIAN INDUSTRIES CORP.
To: GUARDIAN GLASS, LLC
Reel/Frame 044002/0786 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 20, 2017
From: INTERMOLECULAR, INC.
To: GUARDIAN INDUSTRIES CORP.
Reel/Frame 043920/0806 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 12, 2013
From: LIANG, LIANG; BLACKER, RICHARD; KALYANKAR, NIKHIL; JEWHURST, SCOTT
To: GUARDIAN INDUSTRIES CORP.; INTERMOLECULAR, INC.
Reel/Frame 030592/0316 →