Stabilization of titanium oxide films for highly transparent coatings
View Patent ↗A sol-gel material for overcoating a surface-relief structure includes a titanium(IV) precursor, and a titanium oxide stabilizer including R 3 OC(O)OR 4 , R 5 C(O)OR 6 , or a combination. R 3 and R 4 include alkyl or alkene groups optionally containing carboxylate, alcohol, or ester functionalities, such as propylene carbonate (PC). R 5 and R 6 include alkyl or alkene groups optionally containing carboxylate, alcohol, or ester functionalities, for example, a lactone such as gamma butyrolactone (GBL). In some embodiments, the sol-gel material includes a source of sulfate or phosphate anions, an acid, a base, a peroxide, a surfactant, a cross-linker, a flexibilizer, a toughener additive, a solvent, or a combination thereof. In some embodiments, the sol-gel material is annealed at a temperature between 50-150° C., and then annealed at a temperature between 200-300° C. In some embodiments, the sol-gel material is cured using ultraviolet light before annealing at a temperature between 200-300° C.
1. A sol-gel material for overcoating surface-relief structures, the sol-gel material comprising:
a titanium (IV) precursor; and
a titanium oxide stabilizer including R 3 OC(O)OR 4 , R 5 C(O)OR 6 , or a combination,
wherein R 3 , R 4 , R 5 , and R 6 include alkyl or alkene groups, and
wherein the sol-gel material, when coated onto a substrate and annealed at a temperature below about 300° C. for less than about 10 minutes, forms a coating with a refractive index in a range of 1.6-1.9 and an absorption for visible light less than about 0.1% per 100 nm.
2. The sol-gel material of claim 1 , wherein R 3 and R 4 include carboxylate, alcohol, or ester functionalities.
3. The sol-gel material of claim 1 , wherein R 3 and R 4 are parts of a heterocycle.
4. The sol-gel material of claim 1 , wherein the titanium oxide stabilizer includes R 3 OC(O)OR 4 in a range of 0.1-10% by mass of the sol-gel material.
5. The sol-gel material of claim 1 , wherein the titanium oxide stabilizer includes propylene carbonate or a lactone.
6. The sol-gel material of claim 1 , wherein R 5 and R 6 include carboxylate, alcohol, or ester functionalities.
7. The sol-gel material of claim 1 , wherein R 5 and R 6 are parts of a heterocycle.
8. The sol-gel material of claim 1 , wherein the titanium oxide stabilizer includes R 5 C(O)OR 6 in a range of 0.1-50% by mass of the sol- gel material.
9. The sol-gel material of claim 1 , wherein:
the titanium (IV) precursor includes Ti-OR 1 (m) -X (n) , wherein m≥0 and n>0;
R 1 includes an alkyl or alkene group; and
X includes a halide, sulfate, or phosphate.
10. The sol-gel material of claim 1 , wherein the sol-gel material is configured to fill recessed features on the substrate in a superconformal fashion without leading to voiding upon full thermal densification of the sol-gel material.
11. The sol-gel material of claim 1 , further comprising a source of sulfate or phosphate anions, an acid, a base, a peroxide, a surfactant, a cross-linker, a flexibilizer, a toughener additive, a solvent, or a combination thereof.
12. The sol-gel material of claim 1 , further comprising one or more solvents with boiling points greater than 140° C.