Polymeric coatings for fortification of visible, infrared, and laser optical devices

Patent metadata

Field	Value
Publication number	US-9616459-B1
Application number	US-201414549804-A
Country	US
Kind code	B1
Filing date	Nov 21, 2014
Priority date	Apr 17, 2014
Publication date	Apr 11, 2017
Grant date	Apr 11, 2017

Abstract

A method for coating a surface of a material involves contacting a surface of a material with a surface activator containing a fluoride-containing compound and an organic solvent to form an activated surface, contacting the activated surface with a protective reagent to form an initial coated surface, and contacting the initial coated surface with a thinning agent containing a fluoride-containing compound and a surfactant to from a final coated surface, wherein the final coated surface is coated with a protective coating that is covalently bonded to the surface of the material.

First claim

The invention claimed is:

1. A method for producing a covalently bound, monolayer protective coating on the surface of a material, the method comprising:
(i) activating the surface of the material by contacting the surface with a surface activator that increases the concentration of polar binding sites on the surface to form a polar surface, wherein the surface activator comprises an organic solvent and a first fluoride-containing compound selected from the group consisting of barium fluoride (BaF 2 ), hydrogen fluoride (HF), ammonium fluoride (NH 4 F), sodium fluoride (NaF), sodium bifluoride (NaHF 2 ), potassium fluoride (KF), potassium bifluoride (KHF 2 ), ammonium difluoride (NH 4 HF 2 ), any hydrate thereof, and any mixture thereof;
(ii) coating the activated polar surface of (i) with a protective reagent that reacts with the activated surface of (i) to form a covalently bound protective coating; and
(iii) thinning the covalently bound protective coating by contacting the covalently bound protective coating with a thinning agent that removes additional outer layers of coating and contaminants, wherein the thinning agent comprises a surfactant and a second fluoride-containing compound selected from the group consisting of barium fluoride (BaF 2 ), hydrogen fluoride (HF), ammonium fluoride (NH 4 F), sodium fluoride (NaF), sodium bifluoride (NaHF 2 ), potassium fluoride (KF), potassium bifluoride (KHF 2 ), ammonium difluoride (NH 4 HF 2 ), any hydrate thereof, and any mixture thereof;

to form a covalently bound monolayer protective coating on the surface.

2. The method of claim 1 , further comprising:
before the activating step (i), performing a first surface test on the surface of the material in order to detect the presence or absence of a hydrophobic film or substance on the surface of the material; and
after the thinning step (iii), performing a second surface test on the final coated surface in order to detect the presence or absence of a hydrophilic area or substance on the final coated surface.

3. The method of claim 1 , further comprising contacting the surface of the material with a cleaner to clean the surface of the material.

4. The method of claim 3 , wherein the cleaner is an alkaline cleaner.

5. The method of claim 3 , wherein the cleaner comprises at least one selected from the group consisting of a phosphate salt, a silicate salt, a carbonate salt, and a borate salt.

6. The method of claim 3 , wherein the cleaner comprises a sodium silicate.

7. The method of claim 3 , wherein the cleaner is warmed to a predetermined cleaning temperature at which the contacting of the surface of the material with the cleaner occurs.

8. The method of claim 1 , wherein subsequent to (ii) and before (iii), the method comprises drying the covalently bound protective coating for a predetermined drying time period to form a dried covalently bound protective coating and heating the dried covalently bound protective coating at a predetermined drying temperature and at a predetermined drying humidity for a predetermined heating time period.

9. The method of claim 1 , further comprising, before the activating step (i):
(A) contacting the surface of the material with an alkaline cleaner to clean the surface of the material;
(B) performing a first surface test on the surface of the material in order to detect the presence or absence of a hydrophobic film or substance on the surface of the material; and
(C) optionally repeating the contacting step (A) and the performing step (B) until the surface test indicates that the surface of the material is a uniformly hydrophilic surface with no hydrophobic area or substance detected.

10. The method of claim 2 , further comprising repeating coating step (ii), thinning step (iii), and performing the second surface test until the second surface test indicates that the final coated surface is a uniformly hydrophobic surface with no hydrophilic area or substance detected.

11. The method of claim 1 , wherein the surface activator comprises the first fluoride-containing compound, the organic solvent, an acid, an anionic surfactant, and water.

12. The method of claim 1 , wherein the surface activator comprises:
at least one selected from the group consisting of barium fluoride, hydrogen fluoride, ammonium fluoride, sodium fluoride, sodium bifluoride, potassium fluoride, potassium bifluoride, and ammonium difluoride;
at least one selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, hydrobromic acid, hydroiodic acid, chloric acid, perchloric acid, formic acid, acetic acid, trichloroacetic acid, nitrous acid, sodium hydrogen sulfate and potassium hydrogen sulfate;
a polar protic organic solvent or a polar aprotic organic solvent; and
an anionic surfactant.

13. The method of claim 1 , wherein the surface activator comprises water and:
about 0.1 to 10 percent by volume of the first fluoride-containing compound;
about 0.1 to 10 percent by volume of an acid;
about 0.1 to 20 percent by volume of the organic solvent; and
about 0 to 10 percent by volume of an anionic surfactant.

14. The method of claim 1 , wherein the surface activator comprises water and:
about 0.1 to 10 percent by volume of at least one selected from the group consisting of barium fluoride, hydrogen fluoride, ammonium fluoride, sodium fluoride, sodium bifluoride, potassium fluoride, potassium bifluoride, ammonium difluoride;
about 0.1 to 10 percent by volume of at least one selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, hydrobromic acid, hydroiodic acid, chloric acid, perchloric acid, formic acid, acetic acid, trichloroacetic acid, nitrous acid, sodium hydrogen sulfate and potassium hydrogen sulfate;
about 0.1 to 20 percent by volume of at least one selected from the group consisting of methanol, ethanol, formic acid, n-butanol, isopropanol, 2,2,2-tribromoethanol, 2,2,2-trichloroethanol, 2,2,2-trifluoroethanol, 2,2-dichloroethanol, 2-chloroethanol, 2-fluoroethanol, 2-nitroethanol, 1,1,1,3,3,3-hexafluoro-2-propanol, 2,2,3,3,3-pentafluoro-1-propanol, 2,2,3,3-tetrafluoro-1-propanol, 1,1,1-trifluoropropanol, 3,3,3-trifluoro-1-propanol, 1,3-difluoro-2-propanol, 1,3-dichloro-2-propanol, 3-fluoro-1-propanol, 2-pentanol, 2-methyl-1-butanol, 2,2-dimethyl-1-propanol, 2-methyl-1-butanol, 3-methyl-2-butanol, 3-pentanol, 1-ethoxyl-2-propanol, 1-methoxy-2-butanol, 1-methoxy-2-methyl-propanol, 2-isopropoxyethanol, 3-ethoxy-1-propanol, 3-methoxy-1-butanol, 2-butoxyethanol, 1-methoxy-2-butanol, 1-methoxy-2-methyl-2-propanol, 2-isopropoxyethanol, 3-ethoxy-1-propanol, 3-methoxy-1-butanol, 1,1-dimethoxy-2-propanol, 2-(methoxymethoxy)-1-propanol, cyclohexanol, cyclopentanemethanol, 2-methylcyclopentanol, 1-hexanol, 2,3-dimethyl-2-butanol, 2-ethyl-1-butanol, 2-hexanol, 2-methyl-1-pentanol, 2-methyl-2-pentanol, 2-methyl-3-pentanol, 3,3-dimethyl-1-butanol, 3,3-dimethyl-2-butanol, 3-hexanol, 3-methyl-1-pentaol, 3-methyl-2-pentanol, 3-methyl-3-pentanol, 4-methyl-1-pentanol, 4-methyl-2-pentanol, 3-methoxy-3-methyl-1-butanol, 1,1,1,3,3,3-hexafluoro-2-phenyl-2-propanol, 3,5-bus(trifluoromethyl)benzyl alcohol, 2-(trifluoromethyl)phenethyl alcohol, 3-(trifluoromethyl)phenethyl alcohol, 4-(trifluoromethyl)phenethyl alcohol, 2-[4-(trifluoromethoxy)phenyl]ethanol, 2-hydroxymethyl-1,4-benzodioxane, 3,4-(methylenedioxy)phenethyl alcohol, 3-(4-chlorophenyl)1-propanol, 2-phenyl-2-propanol, benzyl alcohol, 3,4-dimethylbenzyl alcohol, 1-phenoxy-2-propanol, 2-(4-methylphenoxy)ethanol, 2-(benzyloxy)ethanol, 2-ethoxy-4-methylphenol, 2-ethoxybenzyl alcohol, 2-methoxy-2-phenylethanol, 2-methoxyphenethyl alcohol, 3

Assignees

• Lockheed Corp

Inventors

• Lohmeier Linda Ann
• Basile Franklin Charles
• Powell Wayne
• Surface Dennis W

Classifications

• B05D3/107

  Post-treatment of applied coatings · CPC title

• G02B1/14

  Protective coatings, e.g. hard coatings · CPC title

• B05D3/007

  After-treatment · CPC title

• B05D2350/00

  Pretreatment of the substrate · CPC title

• B05D2203/35

  Glass · CPC title