Sol-gel based antireflective (AR) coatings with controllable pore size using organic nanocrystals and dendrimers
View Patent ↗Embodiments of the invention relate generally to methods and compositions for forming porous low refractive index coatings on substrates. In one embodiment, a method for forming a porous coating on a substrate is provided. The method comprises coating a substrate with a sol-gel composition, comprising at least one porosity forming agent, wherein the porosity forming agent is selected from at least one of dendrimers and organic nanocrystals and removing the at least one porosity forming agent to form the porous coating. Use of at least one of the dendrimers and organic nanocrystals leads to the formation of stable pores with larger volume fraction in the film. Further, the size and interconnectivity of the pores may be controlled via selection of the organic nanocrystal or dendrimer structure, the total organic nanocrystal or dendrimer molecule fraction, polarity of the organic nanocrystal or dendrimer molecule and solvent, and other physiochemical properties of the gel phase.
1. A method of forming a porous low refractive index coating on a substrate, comprising:
coating a substrate with a sol-gel composition comprising at least one porosity forming agent, wherein the porosity forming agent is selected from, trimethylol propane (TMP)-cored dendrimers, tetracene nanocrystals, and combinations thereof; and
annealing the coated substrate to remove the at least one porosity forming agent to form the porous coating,
wherein annealing the coated substrate to remove the at least one porosity forming agent comprises heating the coated substrate to a temperature equal or greater than 600 degrees Celsius.
2. The method of claim 1 , wherein the annealing the coated substrate comprises heating the coated substrate to a temperature of greater than 600 degrees Celsius.
3. The method of claim 1 , wherein the annealing the coated substrate comprises heating the coated substrate to a temperature between 625 degrees Celsius and 650 degrees Celsius.
4. The method of claim 1 , wherein the at least one porosity forming agent is present in the sol-gel composition in an amount from about 0.1 wt. % to 5 wt. % of the total weight of the sol-gel composition.
5. The method of claim 1 , further comprising:
drying the sol-gel composition coated on the substrate to form a gel on the substrate.
6. The method of claim 1 , wherein the substrate is a glass substrate.
7. The method of claim 1 , wherein the sol-gel composition further comprises a film forming precursor selected from the group comprising: 3-glycidoxypropyltrimethoxysilane (Glymo), octadecyltrimethoxysilane (OTS), propyltriethoxysilane (PTES), (heptadecafluoro) 1,1,2,2-tetrahydrodecyltrimethoxysilane, and combinations thereof.
8. The method of claim 1 , further comprising:
exposing the porous coating to a silane-based solution to improve the hydrophobicity of the porous coating.
9. The method of claim 8 , wherein the silane-based solution comprises a silane selected from the group comprising propyltriethoxysilane (PTES), octadecyltrimethoxysilane (OTS), (heptadecafluoro)-1,1,2,2-tetrahydrodecyltrimethoxysilane, and combinations thereof.
10. The method of claim 1 , further comprising:
exposing the porous coating to a plasma to seal the pores of the porous coating.
11. A method of making a sol-gel system, comprising:
mixing a film forming precursor, an acid or base containing catalyst, water, and an alcohol containing solvent to form a reaction mixture by at least one of a hydrolysis and polycondensation reaction; and
adding at least one porosity forming agent comprising trimethylol propane (TMP)-cored dendrimers, tetracene nanocrystals, or combinations thereof to the reaction mixture.
12. The method of claim 11 , further comprising a stabilizer selected from the group comprising: polyoxyethylene stearyl ether, 3-glycidoxypropyltrimethoxysilane, polyethyleneglycol (PEG), ammonium lauryl sulfate (ALS), dodecyltrimethylammoniumchloride (DTAC), benzoalkonium chloride (BAC), polyalkyleneoxide modified hepta-methyltrisiloxane, and combinations thereof.
13. The method of claim 11 , further comprising:
heating the reaction mixture to between about 50 degrees Celsius and 60 degrees Celsius;
cooling the heated reaction mixture to room temperature; and
adding additional alcohol containing solvent to the cooled reaction mixture prior to the adding at least one porosity forming agent.
14. The method of claim 11 , wherein the film forming precursor is a silane containing precursor or metal alkoxide containing precursor selected from the group comprising: 3-glycidoxypropyltrimethoxysilane (Glymo), octadecyltrimethoxysilane (OTS), propyltriethoxysilane (PTES), (heptadecafluoro) 1,1,2,2-tetrahydrodecyltrimethoxysilane, and combinations thereof.