# US 2014/0154466 A1 · Method of making hydrophobic coated article, coated article including hydrophobic coatings, and/or sol compositions for use in the same > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2014/0154466 A1 - Document ID: US20140154466A1 - Status: Published application - Kind: A1 - Application number: 13/692,160 - Filed: 2012-12-03 - Published: 2014-06-05 - Earliest claimed: 2012-12-03 - Assignees: Guardian Industries Corp. - Applicants: Guardian Industries Corp. - Inventors: Liang LIANG - Web page: https://patentgrep.com/patent/US20140154466A1 ## CPC - C03C 17/30: with silicon-containing compounds - C03C 17/3663: {specially adapted for use as mirrors} - C09D 183/02: Polysilicates - C09D 183/04: Polysiloxanes - C09D 183/06: containing silicon bound to oxygen-containing groups (C09D183/12 takes precedence) - C09D 183/08: containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen - G02B 1/11: Anti-reflection coatings - C03C 2217/29: Mixtures - C03C 2217/76: Hydrophobic and oleophobic coatings - C03C 2217/77: Coatings having a rough surface - C03C 2218/113: by sol-gel processes - C03C 2218/116: by spin-coating, centrifugation - Y10T 428/24355: Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.] - C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS - C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D) - G02B: OPTICAL ELEMENTS, SYSTEMS OR APPARATUS - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract Certain example embodiments relate to a coated article including a coating formed from a sol that has hydrophobic surface properties. The sol may include a mixture of at least two alkylsiloxane chemicals, with the sol potentially being aged for a certain comparatively short amount of time before being wet-applied to a major substrate surface. The application process may also undergo a certain comparatively short curing process to help provide hydrophobic surface properties. The hydrophobic surface properties help provide anti-soiling functions that are advantageous in a variety of applications including, for example, solar mirror applications. ## Claims ### Claim 1 A method of making a coated article comprising a glass substrate supporting a coating, the method comprising: wet-applying a sol, directly or indirectly, on a major surface of the substrate, the sol comprising at least first and second alkylsiloxane chemicals, the first and second alkylsiloxane chemicals having tetra-alkoxysiloxane and tri-alkoxysiloxane structures, respectively; and drying and/or curing the sol to form the coating, wherein the sol is aged for no more than five months prior to the wet-applying. ### Claim 2 (depends on 1) The method of claim 1, wherein the alkylsiloxane chemicals are provided at substantially equal weight percentages. ### Claim 3 (depends on 1) The method of claim 1, wherein the alkylsiloxane chemicals are selected from the group consisting of octyltrimethoxysiloxane (OTMOS), pentyltriethoxysiloxane (PTEOS), 3,3,3-trifluoropropyl trimethoxysiloxane (TFTMOS), tetraethyl orthosilicate (TEOS), and combinations thereof. ### Claim 4 (depends on 1) The method of claim 1, wherein the sol is aged for less than or equal to 1 month prior to the wet-applying. ### Claim 5 (depends on 1) The method of claim 1, wherein the coating has a root mean square roughness of 3-6.5 nm. ### Claim 6 (depends on 1) The method of claim 1, wherein alkylsiloxane chains protrude outwardly from a surface of the coating. ### Claim 7 (depends on 1) The method of claim 1, wherein alkylsiloxane groups are hydrolyzed using an acid catalysis process. ### Claim 8 (depends on 7) The method of claim 7, wherein the hydrolyzed alkylsiloxane groups are partially condensed to form a tetra-cyclic siloxane, providing nucleation sites for further growths to become three-dimensional particles on the coating. ### Claim 9 (depends on 8) The method of claim 8, wherein the three-dimensional particles grow to 1-5 nm in major distance, with a precursor solution pH of 1-8. ### Claim 10 (depends on 1) The method of claim 1, wherein the coating has a refractive index below 1.3 and a thickness of 60-100 nm. ### Claim 11 (depends on 1) The method of claim 1, wherein the coating is cured for less than 25 minutes. ### Claim 12 (depends on 1) The method of claim 1, wherein a water contact angle theta of the coating is greater than about 100 degrees. ### Claim 13 A method of making a coated article comprising a glass substrate supporting a coating, the method comprising: wet-applying a sol, directly or indirectly, on a major surface of the substrate, the sol comprising tetraethyl orthosilicate (TEOS) and octyltrimethoxysiloxane (OTMOS); and drying and/or curing the sol to form the coating; wherein the coating has an initial contact angle of 100-131 degrees. ### Claim 14 (depends on 13) A method of claim 13, wherein the coating has a root mean square roughness of 4-5 nm. ### Claim 15 (depends on 13) The method of claim 13, wherein TEOS and OTMOS are provided in weight percentages in the sol that differ from one another by no more than 5%. ### Claim 16 (depends on 13) The method of claim 13, wherein the sol is aged for no more than about five months prior to the wet-applying. ### Claim 17 (depends on 13) The method of claim 13, wherein the coating has a refractive index of less than 1.3. ### Claim 18 (depends on 17) The method of claim 17, wherein the coating is provided at a thickness of 70-90 nm. ### Claim 19 (depends on 13) The method of claim 13, wherein the coating is cured for less than 15 minutes. ### Claim 20 A method of making a mirror, the method comprising: disposing a thin film coating on a first major surface of the substrate, the thin film coating having a reflectivity of at least about 85%; wet-applying a sol, directly or indirectly, onto the thin film coating, the sol comprising at least first and second alkylsiloxane chemicals, the first and second alkylsiloxane chemicals having tetra-alkoxysiloxane and tri-alkoxysiloxane structures, respectively, the sol having been aged for no more than three months prior to the wet-applying; and drying and/or curing the sol to form an anti-soiling coating that at least initially has a contact angle of greater than 100 degrees. ### Claim 21 (depends on 20) The method of claim 20, wherein reflection from the mirror is no more than 0.15% lower than the reflection would be if no anti-soiling coating were present. ### Claim 22 (depends on 20) The method of claim 20, wherein the alkylsiloxane chemicals are selected from the group consisting of octyltrimethoxysiloxane (OTMOS), pentyltriethoxysiloxane (PTEOS), 3,3,3-trifluoropropyl trimethoxysiloxane (TFTMOS), tetraethyl orthosilicate (TEOS), and combinations thereof. ### Claim 23 (depends on 20) The method of claim 20, wherein the anti-soiling coating has a refractive index of less than 1.3. ### Claim 24 (depends on 23) The method of claim 23, wherein the anti-soiling coating has a thickness of 60-100 nm. ### Claim 25 (depends on 20) The method of claim 20, wherein the anti-soiling coating has a curing time of less than 25 minutes. ### Claim 26 A sol composition, comprising: at least two alkylsiloxane chemicals provided at substantially the same weight percents; wherein a first alkylsiloxane chemical has a tetra-alkoxysiloxane structure, and a second alkylsiloxane chemical has a tri-alkoxysiloxane structure, and wherein the sol composition is aged less than 3 months and has a cure time less than 10 minutes. ### Claim 27 (depends on 26) The sol composition of claim 26, wherein the alkylsiloxane chemicals are selected from the group consisting of octyltrimethoxysiloxane (OTMOS), pentyltriethoxysiloxane (PTEOS), 3,3,3-trifluoropropyl trimethoxysiloxane (TFTMOS), tetraethyl orthosilicate (TEOS, Aldrich), and combinations thereof. ### Claim 28 A coated article, comprising: a multi-layer thin film coating disposed, directly or indirectly, on a first major surface of a substrate, the thin film coating having a reflectivity of at least about 85%; and a wet-applied anti-soiling coating formed from a sol aged for no more than about three months prior to the wet application and comprising tetra-alkoxysiloxane and tri-alkoxysiloxane components at least initially provided in substantially equal weight percents; wherein the anti-soiling coating has an initial contact angle theta greater than 100 degrees, a refractive index less than 1.3, a thickness of 60-100 nm, and a root mean square roughness of 3-6.5 nm.