Process of using microwave deposition of metal oxide onto an organic substrate
The present invention is directed to a process for the preparation of a plane-parallel structure (a platelet-shaped body, or flake), comprising at least one dielectric layer consisting of one or more oxides of a metal selected from groups 3 to 15 of the periodic table, which comprises the steps of: (a) applying a thin film of the dielectric material on a flexible belt, by passing the belt through an aqueous solution of a fluorine scavenger and one or more fluorine containing metal complexes which are the precursors of the desired metal oxide coating; and subjecting said solution to microwave radiation to deposit the metal oxide onto said flexible belt, wherein step (a) can optionally be repeated using different fluorine containing metal complexes to produce one or more metal oxide layers or a gradient of concentration of 2 different metal oxides across the thickness; (b) separating the resulting layer from the flexible belt as plane-parallel structures.
1. A process for the preparation of a plane-parallel structure comprising at least one dielectric layer consisting of one or more oxides of a metal selected from groups 3 to 15 of the periodic table, which comprises the steps of:
(a) applying a thin film of the dielectric material on a flexible belt, by passing the belt through an aqueous solution of a fluorine scavenger and one or more fluorine containing metal complexes which are the precursors of the desired metal oxide coating, which belt absorbs microwave radiation better than the solution; and subjecting said solution to microwave radiation to deposit the metal oxide onto said flexible belt, wherein the aqueous solution of the fluorine containing metal complex is added continuously in order that the metal oxide grows on the belt rather than precipitate into bulk of the reaction medium,
wherein step (a) can optionally be repeated using different fluorine containing metal complexes to produce one or more metal oxide layers or a gradient of concentration of 2 different metal oxides across the thickness;
(b) separating the resulting layer from the flexible belt as plane-parallel structures.
2. The process according to claim 1 , wherein the flexible belt is a continuous flexible belt.
3. The process according to claim 2 , wherein the continuous flexible belt is coated with a separating agent before step (a) and (b) separating the resulting layer from the flexible belt is achieved by dissolving the separating agent in a suitable solvent.
4. The process according to claim 1 , wherein the fluorine scavenger is selected from the group consisting of boric acid, an alkali metal borate, ammonium borate, boron anhydride and boron monoxide.
5. The process according to claim 1 ,wherein the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate; ammonium hexaflurostanate; ammonium hexafluorosilicate; iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; aluminum(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; ammonium hexafluorogermanate; indium(III) fluoride, hydrofluoric acid and ammonium fluoride mixtures; and combinations of indium(III) fluoride trihydrate and ammonium hexafluorostanate.
6. The process according to claim 1 , wherein the metal oxide is titanium dioxide and the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate, a complex prepared from ammonium fluoride and titanium chloride or titanium chloride, ammonium fluoride and hydrogen fluoride, or the metal oxide is iron oxide and the fluorine containing metal complex is selected from the group iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures.
7. The process according to claim 1 , wherein the metal oxide is silicon dioxide and the fluorine containing metal complex is ammonium hexafluorosilicate or ammonium pentafluorosilicate.
8. The process according to claim 3 , wherein the fluorine containing metal complex of step (a) is ammonium hexafluorotitanate, an ammonium fluorosilicate salt, or iron(III) chloride/ammonium fluoride, wherein after dissolving of the separating agent in an organic liquid, plane-parallel structures of TiO 2 , SiO 2 , or Fe 2 O 3 are produced.
9. The process of claim 3 further comprising the step of:
(a′) passing the belt through an aqueous solution of a fluorine scavenger and one or more fluorine containing metal complexes which are the precursors of the desired metal oxide coating which is different from the oxide coating in step (a); and subjecting said solution to microwave radiation to deposit the metal oxide onto said flexible belt, wherein step (a′) is conducted after step (a).
10. The process according to claim 9 , wherein step (a) and /or (a′) are repeated to form multilayer plane-parallel structures having alternating layers of metal oxides.
11. The process according to claim 1 , wherein the fluorine scavenger is sodium borate.
12. The process according to claim 3 , wherein the fluorine scavenger is selected from the group consisting of boric acid, an alkali metal borate, ammonium borate, boron anhydride and boron monoxide.
13. The process according to claim 3 , wherein the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate; ammonium hexaflurostanate; ammonium hexafluorosilicate; iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; aluminum(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; ammonium hexafluorogermanate; indium(III) fluoride, hydrofluoric acid and ammonium fluoride mixtures; and combinations of indium(III) fluoride trihydrate and ammonium hexafluorostanate.
14. The process according to claim 4 , wherein the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate; ammonium hexaflurostanate; ammonium hexafluorosilicate; iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; aluminum(III) chloride, hydrofluoric acid and ammonium fluoride mixtures; ammonium hexafluorogermanate; indium(III) fluoride, hydrofluoric acid and ammonium fluoride mixtures; and combinations of indium(III) fluoride trihydrate and ammonium hexafluorostanate.
15. The process according to claim 3 , wherein the metal oxide is titanium dioxide and the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate, a complex prepared from ammonium fluoride and titanium chloride or titanium chloride, ammonium fluoride and hydrogen fluoride, or the metal oxide is iron oxide and the fluorine containing metal complex is selected from the group iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures.
16. The process according to claim 4 , wherein the metal oxide is titanium dioxide and the fluorine containing metal complex is selected from the group consisting of ammonium hexafluorotitanate, a complex prepared from ammonium fluoride and titanium chloride or titanium chloride, ammonium fluoride and hydrogen fluoride, or the metal oxide is iron oxide and the fluorine containing metal complex is selected from the group iron(III) chloride, hydrofluoric acid and ammonium fluoride mixtures.
17. The process according to claim 3 , wherein the metal oxide is silicon dioxide and the fluorine containing metal complex is ammonium hexafluorosilicate or ammonium pentafluorosilicate.
18. The process according to claim 4 , wherein the metal oxide is silicon dioxide and the fluorine containing metal complex is ammonium hexafluorosilicate or ammonium pentafluorosilicate.
19. The process of claim 10 , wherein the multilayer plane-parallel structures have alternating layers of metal oxides A/A′/A, or A/A′/A/A′/A/A′/A, wherein A, the metal oxide layer obtained in step (a), is TiO 2 , and A′, the metal oxide layer obtained in step (a′), is SiO 2 ; or the multilayer plane-parallel structures have alternating layers of metal oxides B/B′/B/B′/B, wherein B the metal oxide layer obtained in step (a), is SiO 2 , and B′, the metal oxide layer obtained in step (a′), is TiO 2 .