Multilayer heterostructures and their manufacture
A method of synthesizing multilayer heterostructures including an inorganic oxide layer residing on a solid substrate is described. Exemplary embodiments include producing an inorganic oxide layer on a solid substrate by a liquid coating process under relatively mild conditions. The relatively mild conditions include temperatures below 225° C. and pressures above 9.4 mb. In an exemplary embodiment, a solution of diethyl aluminum ethoxide in anhydrous diglyme is applied to a flexible solid substrate by slot-die coating at ambient atmospheric pressure, and the diglyme removed by evaporation. An AlO x layer is formed by subjecting material remaining on the solid substrate to a relatively mild oven temperature of approximately 150° C. The resulting AlO x layer exhibits relatively high light transmittance and relatively low vapor transmission rates for water. An exemplary embodiment of a flexible solid substrate is polyethylene napthalate (PEN). The PEN is not substantially adversely affected by exposure to 150° C.
1. A method comprising:
providing an organometallic solution, the organometallic solution including an organometallic compound dissolved in a complexing solvent;
distributing the organometallic solution on a solid substrate, wherein the solid substrate comprises an organic polymer and the distributing is by a first liquid coating process;
removing the complexing solvent; and
curing the organometallic compound to form a metallic oxide from the organometallic compound, wherein the metallic oxide produces a first metal oxide layer on the solid substrate.
wherein the distributing is by a liquid coating process.
2. The method of claim 1 , wherein the organometallic solution includes a water content of less than 500 ppm.
3. The method of claim 1 , wherein the solid substrate is flexible at 20° C., being capable of bending 90° around a curve having a radius of 0.5 inch or less without apparent fracturing.
4. The method of claim 1 , wherein the distributing, the removing, and the curing are performed at a temperature under 225° C. and a processing pressure greater than 9.4 mb.
5. The method of claim 4 , wherein the processing pressure is greater than 475 mb.
6. The method of claim 4 , wherein the processing pressure is greater than 800 mb.
7. The method of claim 1 , wherein the distributing, the removing, and the curing are performed at about ambient atmospheric pressure.
8. The method of claim 7 , wherein the distributing, the removing, and the curing are performed at a temperature of 225° C. or less.
9. The method of claim 8 , further comprising producing a first organic polymer layer on the first metal oxide layer by a second liquid coating process.
10. The method of claim 9 , wherein the second liquid coating process for producing the first organic polymer layer comprises:
providing an organic polymer solution, the organic polymer solution including an organic polymer dissolved in an organic solvent;
distributing the organic polymer solution on the first metal oxide layer at a process pressure of about ambient atmospheric pressure; and
removing the organic solvent.
11. The method of claim 10 , further comprising distributing the organometallic solution on the first organic polymer layer and producing a second metal oxide layer on the first organic polymer layer.
12. The method of claim 10 , wherein the organic polymer layer comprises polymethylmethacrylate and the organic solvent comprises at least one of dichloromethane, methyl ethyl ketone, or ethyl acetate.
13. The method of claim 1 , wherein the organometallic compound comprises a Lewis acid and the complexing solvent comprises a Lewis base.
14. The method of claim 13 , wherein the Lewis acid comprises at least one of diethylaluminum ethoxide, polymethylsilsesquiloxane, diethyl zinc, titanium diisopropoxide, polydiethoxysiloxane, or polymethylhydridosiloxane.
15. The method of claim 13 , wherein the Lewis acid comprises at least one of diethylene glycol, dimethyl ether, diethyl ether, tetrahydrofuran, pyridine, acetonitrile, tetramethylethylenediamine, or tris(pentafluorophenyl)borane.
16. The method of claim 1 , wherein the metal oxide layer comprises at least one of SnO x ,InZnO x , or SiO x .
17. A method comprising:
providing an organometallic solution, the organometallic solution including an organometallic compound dissolved in a complexing solvent;
distributing the organometallic solution on a solid substrate at about ambient atmospheric pressure;
removing the complexing solvent at a temperature of 225° C. or less;
curing the organometallic compound to form a metallic oxide from the organometallic compound, wherein the metallic oxide forms a first metal oxide layer on the solid substrate at a temperature of 225° C. or less;
producing a first organic polymer layer on the first metal oxide layer by a first liquid coating process, the first liquid coating process comprising:
providing an organic polymer solution, the organic polymer solution including an organic polymer dissolved in a solvent;
distributing the organic polymer solution on the first metal oxide layer about ambient atmospheric pressure; and
removing the solvent;
distributing the organometallic solution on the first organic polymer layer at about ambient atmospheric pressure;
curing the organometallic compound to form a metallic oxide from the organometallic compound, wherein the metallic oxide forms a second metal oxide layer on the first organic polymer layer at a temperature of 225° or less; and
producing a second organic polymer layer on the second metal oxide layer by the first liquid coating process,
wherein the distributing of the organometallic solution is by a second liquid coating process.
18. A method comprising:
providing a solution, the solution including an organometallic compound dissolved in a complexing solvent, and less than 1000 ppm water;
distributing the solution on a flexible solid substrate at a process pressure of greater than 475 mb;
removing the complexing solvent;
curing the organometallic compound to form a metallic oxide from the organometallic compound, wherein the metallic oxide forms a metal oxide layer on the solid substrate;
producing an organic polymer layer on the metal oxide layer by a first liquid coating process, the first liquid coating process including:
providing an organic polymer solution, the organic polymer solution including an organic polymer dissolved in a solvent;
distributing the organic polymer solution on the metal oxide layer at a process pressure of greater than 475 mb; and
removing the solvent,
wherein the distributing of the solution including an organometallic compound dissolved in a complexing solvent is by a second liquid coating process.
19. A method comprising:
producing an inorganic oxide layer on a solid substrate by a first liquid coating process, the first liquid coating process comprises applying an organometallic solution that includes an organometallic compound dissolved in a complexing agent, followed by curing of the organometallic compound to form a metallic oxide from the organometallic compound, wherein the metallic oxide forms the inorganic oxide layer having a thickness of 200 nm or less; and
producing an organic polymer layer on the inorganic oxide layer by a second liquid coating process at a process pressure greater than 9.4 mb.
20. The method of claim 19 , wherein the organometallic solution comprises a reactive organosilicon compound and curing results from removing the complexing agent.
21. The method of claim 20 , wherein:
the inorganic oxide layer comprises SiO x ;
the applying, the curing, and the producing are performed at about ambient atmospheric pressure.
22. A method comprising:
producing an SiO x layer on a solid substrate by a first liquid coating process, the solid substrate being capable of bending 90° around a curve having a radius of 3.0 inches or less at 20° C. without apparent fracturing, the SiO x layer having a thickness of 200 nm or less, and the first liquid coating process including:
providing a first blend, the first blend including a first complexing solvent combined with a first organosilicon compound;
distributing the first blend on the solid substrate at about ambient atmospheric pressure;
forming a first inorganic oxide layer comprising the SiO x layer by curing the first organosilicon compound by removing the first complexing solvent;
producing a first organic polymer layer on the SiO x layer by a second liquid coating process, the second liquid coating process including:
providing a first organic polymer solution, the first organic polymer solution including a first organic polymer dissolved in a first solvent;
distributing the first organic polymer solution on the SiO x layer at about ambient atmospheric pressure;
forming a second inorganic oxide layer on the first organic polymer layer by a third liquid coating process, the third liquid coating process including:
providing a second blend, the second blend including a second complexing solvent combined with a second organosilicon compound or an organometallic compound;
distributing the second blend on the first organic polymer layer at about ambient atmospheric pressure,
wherein the second inorganic oxide layer comprises either a second SiO x layer or a non-SiO x metal oxide layer, formed by curing either the second organosilicon or the organometallic compound by removing the second complexing solvent;
producing a second organic polymer layer on the second inorganic oxide layer by a fourth liquid coating process, the fourth liquid coating process including:
providing a second organic polymer solution, the second organic polymer solution including a second organic polymer dissolved in a second solvent; and
distributing the second organic polymer solution on the second inorganic oxide layer at about ambient atmospheric pressure,
wherein producing the second organic polymer layer on the second inorganic oxide layer is by a fourth liquid coating process.