Composition and process for making a porous inorganic oxide coating
View Patent ↗The invention relates to a coating composition for making a porous inorganic oxide coating layer on a substrate, the composition comprising an inorganic oxide precursor as binder, a solvent, and a synthetic polyampholyte as pore forming agent. The size of the pores in the coating can be advantageously controlled by the comonomer composition of the polyampholyte, and/or by selecting conditions like temperature, pH, salt concentration, and solvent composition when making the composition. The invention also relates to a method of making such coating composition, to a process of applying a coating on a substrate using such composition, and to such coated substrate showing a specific combination of optical and mechanical properties.
1. A coating composition for making a porous inorganic oxide coating on a substrate, the coating composition comprising an inorganic oxide precursor as a binder, a solvent, and dispersed colloidal particles of an organic synthetic polyampholyte as a pore forming agent, wherein the organic synthetic polyampholyte is a copolymer of at least one comonomer having a positively charged group, at least one comonomer having a negatively charged group and optionally at least one neutral comonomer.
2. The coating composition according to claim 1 , wherein the inorganic oxide precursor is at least one compound selected from the group of metal salts, metal chelates and organo-metallic compounds of Si, Al, Ti, Ta, and Zr.
3. The coating composition according to claim 2 , wherein the inorganic oxide precursor comprises an alkoxy silane.
4. The coating composition according to claim 1 , wherein the polyampholyte is an addition copolymer made from vinyl monomers.
5. The coating composition according to claim 1 , wherein the polyampholyte is a copolymer of:
at least one cationic or basic monomer (M1), including compounds with a pending group that can combine with a proton;
at least one anionic or acidic monomer (M2), including compounds with a pending group that can yield a proton;
at least one neutral or non-ionic monomer (M3); and
optionally at least one cross-linking monomer (M4).
6. The coating composition according to claim 5 , wherein the polyampholyte is a cationic copolymer of:
5-40 mole % of at least one monomer M1;
0.5-20 mole % of at least one monomer M2;
38-94.5 mole % of at least one monomer M3; and
02mole % of at least one monomer M4.
7. The coating composition according to claim 5 , wherein the polyampholyte is a cationic copolymer of:
8-20 mole % of at least one monomer M1 selected from the group consisting of amino-functional (meth)acrylates and (meth)acrylamides;
1-4 mole % of at least one monomer M2 selected from the group of (meth)acrylic monomers with a carboxylic acid group; and
76-91 mole % of at least one monomer M3 selected from the group of C1-C18 alkyl (meth)acrylates.
8. The coating composition according to claim 1 , wherein the polyampholyte particles have an average size of 20-200 nm as measured with dynamic light scattering (DLS).
9. The coating composition according to claim 5 , wherein the basic monomer (M1) includes monomers with a tertiary amine group.
10. The coating composition according to claim 5 , wherein the acidic monomer (M2) includes monomers containing carboxylic acid groups.
11. A method of making the coating composition according to claim 1 , comprising the steps of:
a) providing an aqueous dispersion of colloidal particles of the synthetic polyampholyte; and
b) adding at least one inorganic oxide precursor.
12. The method according to claim 11 , wherein step a) comprises dispersing the synthetic polyampholyte in an aqueous medium, and adjusting particle size by changing both pH and temperature.
13. The method according to claim 11 , further comprising a step c) of stabilising the dispersion obtained by changing the pH to a level at which the inorganic oxide precursor and its reaction products will not react.
14. A process for making an anti-reflective coated transparent substrate comprising the steps of:
(i) applying the coating composition according to claim 1 to a surface of a substrate; and
(ii) drying and curing the applied coating layer to form an anti-reflective coated transparent substrate.
15. The process according to claim 14 , wherein the substrate is an inorganic glass, and wherein curing is performed by heating at temperatures above a decomposition temperature of the polyampholyte.
16. An anti-reflective (AR) coated transparent substrate which comprises a transparent substrate, and a dried and cured layer of the coating composition according to claim 1 on the substrate.
17. The AR coated transparent substrate of claim 16 , which exhibits a minimum reflection in a wavelength range 425-675 nm of at most 1% and a pencil hardness of at least 4H according to ASTM D3363 with a nominal load 300 g.