Light-emitting device
US-2024361583-A1 · Oct 31, 2024 · US
US9545161B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9545161-B2 |
| Application number | US-16064407-A |
| Country | US |
| Kind code | B2 |
| Filing date | Feb 12, 2007 |
| Priority date | Feb 14, 2006 |
| Publication date | Jan 17, 2017 |
| Grant date | Jan 17, 2017 |
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The invention relates to an article comprising a substrate and a nano-porous coating, wherein the reflectivity of the article is less then 2%, and whereby the amount of sodium measured in the coating by XPS is less then 1 wt %, and further to a method of making the article.
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The invention claimed is: 1. A method of making an article with anti-reflective properties comprising the steps of: (i) reacting nano-particles with an amount of surface modifying agent; (ii) pre-hydrolysing an inorganic binder; (iii) mixing the surface modified particles from step (i) with the pre-hydrolysed binder from step (ii) to form a coating composition; (iv) applying the coating composition to a substrate that includes hygroscopic sodium salt compounds; (v) forming a cured coating by curing the coating composition and causing the hygrosopic sodum salt compounds to migrate into the cured coating at a curing temperature of between about 200° C. to about 700° C. and causing the hygroscopic sodium salt compounds to migrate into the cured coating; (vi) washing the cured coating with water or a solvent for the hygroscopic sodium salt compounds for about 30 seconds sufficient to remove the hygroscopic sodium salt compounds from the cured coating and thereby obtain an article having a reflectivity of less than 2% after storage for 28 days and having an amount of sodium measured in the coating by XPS of less than 1 wt %. 2. The method according to claim 1 , wherein the curing temperature of step (v) is between 200° C. and 500° C. 3. The method according to claim 1 , wherein the reflectivity of the article is less than 1%. 4. The method according to claim 1 , wherein the substrate is glass. 5. The method according to claim 4 , wherein the substrate comprises between 0 and 7 wt % of sodium oxide. 6. The method according to claim 1 , which further comprises providing a blocking layer between the coating and the substrate. 7. The method according to claim 6 , wherein the blocking layer comprises CeO 2 . 8. The method according to claim 1 , wherein the coating has an arithmetic average roughness of about 2 to about 50 nm. 9. A method of making an article with anti-reflective properties comprising the steps of: (i) forming a coating composition by reacting nano-particles with an inorganic binder selected from the group consisting of alkoxy silanes, alkoxy zirconates, alkoxy aluminates, alkoxy titanates, alkyl silicates, sodium silicates and mixtures thereof; (ii) applying the coating composition to a substrate that includes hygroscopic sodium salt compounds; (iii) obtaining a cured coating by curing the applied coating composition at a curing temperature between about 200° C. to about 700° C. to form a porous coating and causing the hygroscopic sodium salt compounds to migrate into the cured coating; and (iv) washing the cured coating with water or a solvent for the hygroscopic sodium salt compounds for about 30 seconds sufficient to remove the hygroscopic sodium salt compounds and thereby obtain an article having a reflectivity of less than 2% after storage for 28 days and having an amount of sodium measured in the coating by XPS of less than 1 wt %. 10. The method according to claim 9 , wherein the curing temperature of step (iii) is between 200° C. and 500° C. 11. The method according to claim 9 , wherein the reflectivity of the article is less than 1%. 12. The method according to claim 9 , wherein the substrate is glass. 13. The method according to claim 12 , wherein the substrate comprises between 0 and 7 wt % of sodium oxide. 14. The method according to claim 9 , which further comprises providing a blocking layer between the coating and the substrate. 15. The method according to claim 14 , wherein the blocking layer comprises CeO 2 . 16. The method according to claim 9 , wherein the coating has an arithmetic average roughness of about 2 to about 50 nm. 17. The method according to claim 9 , wherein the inorganic binder is tetra alkoxy silane. 18. The method according to claim 9 , wherein the inorganic binder is present in the coating composition in an amount of 1% to 40%, by weight of solids. 19. The method according to claim 9 , wherein step (iv) comprises drying the cured coating in ambient air for about 1 hour after washing. 20. The method according to claim 9 , wherein step (iv) is practiced by washing the cured coating with a dilute acid solvent for hygroscopic salt compounds selected from the group consisting of formic acid, acetic acid, benzoic acid, sulphuric acid, nitric acid, hydrochloric acid and phosphoric acid.
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