Nonaqueous sol-gel for adhesion enhancement of water-sensitive materials
US-2019002705-A1 · Jan 3, 2019 · US
US10926237B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10926237-B2 |
| Application number | US-201816226992-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 20, 2018 |
| Priority date | Feb 2, 2018 |
| Publication date | Feb 23, 2021 |
| Grant date | Feb 23, 2021 |
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Aspects described herein generally relate to a sol-gel that is the reaction product of an organosilane, a metal alkoxide, an acid, and chromium (III) salt and/or a lanthanide salt having a solubility of about 1 gram or greater per gram of sol-gel at 23° C. The lanthanide salt includes a cation and a ligand. The cation can be lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium, cobalt, calcium, strontium, barium, and zirconium. A ligand can be a nitrate, a trifluoromethane sulfonate, a sulfate, a phosphate, a hydroxide, or hydrate forms thereof. The chromium (III) salt includes a cation and a ligand. The cation is chromium (III) and the ligand can be a nitrate, a trifluoromethane sulfonate, a sulfate, a phosphate, a hydroxide, or hydrate forms thereof.
Opening claim text (preview).
What is claimed is: 1. A sol-gel comprising: an organosilane a metal alkoxide; an acid; a chromium (III) salt comprising a ligand selected from a nitrate, a trifluoromethane sulfonate, a sulfate, a phosphate, a hydroxide, or hydrate forms thereof; and water. 2. The sol-gel of claim 1 , wherein a weight fraction of the chromium (III) salt in the sol-gel is about 0.2 wt % to about 50 wt %. 3. The sol-gel of claim 1 , wherein a ratio of chromium (III) salt to the sum of metal alkoxide, organosilane, and acid is about 0.01:1 to about 0.5:1 by weight. 4. The sol-gel of claim 1 , wherein a ratio of chromium (III) salt to (metal alkoxide+organosilane+acid) is about 1:1 to about 5:1 by weight. 5. The sol-gel of claim 1 , wherein the sol-gel has a solids content of about 1 wt % or less, based on the total weight of the sol-gel. 6. The sol-gel of claim 5 , wherein the sol-gel has a halogen content of about 1 wt % or less, based on the total weight of the sol-gel. 7. The sol-gel of claim 6 , wherein the sol-gel comprises about 80 wt % or greater of water. 8. The sol-gel of claim 6 , wherein the organosilane is represented by Formula (I): wherein: each R 1 is independently selected from C 1 -C 20 alkyl; and R 2 is selected from alkyl, cycloalkyl, ether, and aryl. 9. The sol-gel of claim 6 , wherein the organosilane is represented by Formula (II): wherein R is selected from alkyl, cycloalkyl, ether, and aryl. 10. The sol-gel of claim 9 , wherein the organosilane is: 11. The sol-gel of claim 1 , wherein the metal alkoxide is selected from zirconium (IV) tetramethoxide, zirconium (IV) tetraethoxide, zirconium (IV) tetra-n-propoxide, zirconium (IV) tetra-isopropoxide, zirconium (IV) tetra-n-butoxide, zirconium (IV) tetra-isobutoxide, zirconium (IV) tetra-n-pentoxide, zirconium (IV) tetra-isopentoxide, zirconium (IV) tetra-n-hexoxide, zirconium (IV) tetra-isohexoxide, zirconium (IV) tetra-n-heptoxide, zirconium (IV) tetra-isoheptoxide, zirconium (IV) tetra-n-octoxide, zirconium (IV) tetra-n-isooctoxide, zirconium (IV) tetra-n-nonoxide, zirconium (IV) tetra-n-isononoxide, zirconium (IV) tetra-n-decyloxide, zirconium (IV) tetra-n-isodecyloxide, or mixtures thereof. 12. The sol-gel of claim 1 , wherein the acid is acetic acid. 13. The sol-gel of claim 1 , wherein a weight fraction of the sum of metal alkoxide, organosilane, and acid in the sol-gel is at least 4 wt %. 14. The sol-gel of claim 13 , wherein the weight fraction is at least 15 wt %. 15. The sol-gel of claim 1 , wherein the chromium (III) salt comprises a sulfate ligand or hydrate form thereof. 16. The sol-gel of claim 15 , wherein the chromium (III) salt is chromium (III) sulfate hexahydrate. 17. The sol-gel of claim 1 , wherein the chromium (III) salt comprises a nitrate ligand or hydrate form thereof. 18. The sol-gel of claim 1 , wherein the chromium (III) salt comprises a trifluoromethane sulfonate ligand or hydrate form thereof. 19. The sol-gel of claim 1 , wherein the chromium (III) salt comprises a phosphate ligand or hydrate form thereof. 20. The sol-gel of claim 1 , wherein the chromium (III) salt comprises a hydroxide ligand or hydrate form thereof. 21. A component comprising: a metal substrate; and the sol-gel of claim 1 disposed on the metal substrate. 22. The component of claim 21 , further comprising a secondary layer disposed on the sol-gel. 23. The component of claim 22 , wherein the secondary layer is an epoxy coating or urethane coating. 24. The component of claim 21 , wherein the component is a vehicle component selected from an auxiliary power unit, a nose of an aircraft, a fuel tank, a tail cone, a panel, a coated lap joint between two or more panels, a wing-to-fuselage assembly, a structural aircraft composite, a fuselage body-joint, a wing rib-to-skin joint, or an internal component. 25. The component of claim 21 , wherein the metal substrate comprises a metal selected from aluminum, aluminum alloy, nickel, iron, iron alloy, steel, titanium, titanium alloy, copper, copper alloy, or mixtures thereof. 26. A method of forming a sol-gel, comprising: mixing a metal alkoxide and an acid to form a first mixture; mixing with the first mixture an organosilane to form a second mixture; and mixing a chromium (III) salt with the second mixture to form a third mixture, wherein the chromium (III) salt comprises a ligand selected from a nitrate, a trifluoromethane sulfonate, a sulfate, a phosphate, a hydroxide, or hydrate forms thereof. 27. The method of claim 26 , further comprising depositing the third mixture onto a metal substrate. 28. The method of claim 27 , further comprising curing the third mixture. 29. The method of claim 27 , further comprising cleaning the metal substrate by degreasing, alkaline washing, chemical etching, chemically deoxidizing, and/or mechanically deoxidizing the metal substrate prior to depositing. 30. The method of claim 27 , further comprising depositing a secondary layer onto the sol-gel. 31. The method of claim 26 , wherein the chromium (III) salt comprises a sulfate ligand or hydrate form thereof. 32. The method of claim 31 , wherein the chromium (III) salt is a chromium (III) sulfate hexahydrate. 33. The method of claim 26 , wherein the chromium (III) salt comprises a nitrate ligand or hydrate form thereof. 34. The method of claim 26 , wherein the chromium (III) salt comprises a trifluoromethane sulfonate ligand or hydrate form thereof. 35. The method of claim 26 , wherein the chromium (III) salt comprises a phosphate ligand or hydrate form thereof. 36. The method of claim 26 , wherein the chromium (III) salt comprises a hydroxide ligand or hydrate form thereof.
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