# US 2022/0033971 A1 · Device containing metal oxide-containing layers

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- Number: US 2022/0033971 A1
- Document ID: US20220033971A1
- Status: Published application
- Kind: A1
- Application number: 16/613,970
- Filed: 2018-05-23
- Published: 2022-02-03
- Earliest claimed: 2017-06-01
- Assignees: Evonik Operations GmbH
- Applicants: Evonik Operations GmbH
- Inventors: Jürgen Steiger; Alexey Merkulov; Ralf Anselmann; Gerhard Renner
- Web page: https://patentgrep.com/patent/US20220033971A1

## CPC

- C23C 18/1216: {Metal oxides (C23C18/1212 takes precedence)}
- C09D 1/00: Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D 7/61: inorganic
- C23C 18/1233: {Organic substrates}
- C23C 18/127: {Preformed particles}
- C23C 18/1295: {with after-treatment of the deposited inorganic material}
- H10F 77/1433: {Quantum dots}
- H10K 71/12: using liquid deposition, e.g. spin coating
- H10K 71/15: characterised by the solvent used
- H10K 71/40: Thermal treatment, e.g. annealing in the presence of a solvent vapour
- B82Y 20/00: Nanooptics, e.g. quantum optics or photonic crystals
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- H10K 50/115: comprising active inorganic nanostructures, e.g. luminescent quantum dots
- H10K 50/16: Electron transporting layers
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- H10F: INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

The present invention is directed to process for preparing a device comprising a first layer and a first electrode, the method comprising forming the first layer over a first electrode by applying a liquid anhydrous composition comprising at least one metal oxo alkoxide and at least one solvent, onto a surface, the surface being selected from the surface of the first electrode or the surface of a layer being located over the first electrode, optionally drying the composition, and converting the composition to a metal oxide-containing first layer, and forming a second electrode over the first device layer, wherein the method further includes forming a layer comprising quantum dots over the first electrode before or after the formation of the first layer and to the device itself.

## Claims

### Claim 1

A process for preparing a device comprising a first layer and a first electrode, the process comprising a step forming the first layer over a first electrode by applying a liquid anhydrous composition comprising
i) at least one metal oxo alkoxide of formula (I)
MxOy(OR)z[O(R′O)cH]zXb[R″OH]d (I)
where x=3 to 25,
y=1 to 10,
z=3 to 50,
a=0 to 25,
b=0 to 20,
c=0 to 1,
d=0 to 25,
and M=In, Zn, Ga, Y, Sn, Ge, Sc, Ti, Zr, Al, W, Mo, Ni, Cr, Fe, Hf, Ta, Nb and/or Cu, R, R′, R″=same or different organic radicals, and X=F, Cl, Br, I and
ii) at least one solvent,
onto a surface, the surface being selected from the surface of the first electrode or the surface of a layer being located over the first electrode, drying the composition, and converting the composition to a metal oxide-containing first layer, and forming a second electrode over the first device layer, wherein the method further includes forming a layer comprising quantum dots over the first electrode before or after the formation of the first layer.

### Claim 2 (depends on 1)

The process according to claim 1, characterized in wherein the at least one metal oxo alkoxide used is an oxo alkoxide of the formula MxOy(OR)z where x=3 to 20, y=1 to 8, z=3 to 25, and OR same or different C1-C15-alkoxy, -oxyalkylalkoxy, -aryloxy- or -oxyarylalkoxy groups.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the at least one metal oxo alkoxide of formula (I) is [In5(μ5-O)(μ3-OiPr)4(μ2-OiPr)4(OiPr)5], [Sn3O(OiBu)10(iBuOH)2] and or [Sn6O4(OR)4].

### Claim 4 (depends on 1)

The process according to claim 1, wherein the at least one metal oxo alkoxide is the sole metal oxide precursor used in the process.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the at least one metal oxo alkoxide of formula (I) is present in proportions of 0.1 to 15% by weight, based on the total mass of the anhydrous composition.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the at least one solvent is an aprotic or weakly protic solvent.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the at least one solvent was selected from the group consisting of methanol, ethanol, isopropanol, tetrahydrofurfuryl alcohol, tert-butanol and toluene.

### Claim 8 (depends on 1)

The process according to claim 1, wherein the composition has a viscosity of 1 mPa·s to 10 Pa·s.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the anhydrous composition is applied to the surface by means of a printing process, a spraying process, a rotary coating process, a dipping process, or a process selected from the group consisting of meniscus coating, slit coating, slot-die coating and curtain coating.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the conversion is effected thermally by means of temperatures greater than 80° C.

### Claim 11 (depends on 10)

The process according to claim 10, wherein UV, IR or VIS radiation is applied before, during or after the thermal treatment.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the layer comprising quantum dots is deposited before the formation of the first layer.

### Claim 13 (depends on 1)

The process according to claim 1, wherein the layer comprising quantum dots is deposited after the formation of the first layer.

### Claim 14 (depends on 1)

The process according to claim 1, wherein the process further comprises forming a second layer before or after formation of a layer comprising quantum dots, such that the layer comprising quantum dots is disposed between the first and second layers.

### Claim 15 (depends on 1)

The process to claim 1, wherein the first electrode is deposited on a substrate.

### Claim 16

A device comprising a first layer formed over a first electrode, the first layer comprising a metal oxide formed from a liquid anhydrous composition containing at least one metal oxide precursor, a second electrode over the first layer, and a layer comprising quantum dots disposed between the first layer and one of the two electrodes.

### Claim 17 (depends on 16)

The device according to claim 16, wherein the device is a light-emitting device or is part of a light-emitting device.

### Claim 18 (depends on 16)

The device according to claim 16, wherein the metal oxide comprises indium oxide, zinc oxide, gallium oxide, yttrium oxide, tin oxide, germanium oxide, scandium oxide, titanium oxide, zirconium oxide, aluminum oxide, wolfram oxide, molybdenum oxide, nickel oxide, chromium oxide, iron oxide, hafnium oxide, tantalum oxide, niobium oxide or copper oxide, or mixtures thereof.

### Claim 19 (depends on 16)

The device according to claim 16, wherein the first electrode is deposited onto a substrate.

### Claim 20 (depends on 16)

The device according to claim 16, wherein the first layer is a charge transport layer.

### Claim 21 (depends on 16)

The device according to claim 16, wherein the device further includes a second layer, wherein a layer comprising quantum dots is disposed between the first and second layers.

### Claim 22 (depends on 1)

A device comprising a first layer formed over a first electrode, the first layer comprising a metal oxide formed from a liquid anhydrous composition containing at least one metal oxide precursor, a second electrode over the first layer, and a layer comprising quantum dots disposed between the first layer and one of the two electrodes prepared in accordance with a process according to claim 1.

### Claim 23 (depends on 1)

The process according to claim 1, wherein the at least one metal oxo alkoxide used is an oxo alkoxide of the formula MxOy(OR)z where x=3 to 15, y=1 to 5, z=10 to 20, and OR same or different —OCH3, —OCH2CH3, —OCH2CH2OCH3, —OCH(CH3)2 or —OC(CH3)3.

### Claim 24 (depends on 1)

The process to claim 1, wherein the first electrode is deposited on a substrate.

### Claim 25 (depends on 1)

The process to claim 1, wherein the first electrode is deposited on a semiconductor.

### Claim 26 (depends on 1)

The process to claim 1, wherein the first electrode is deposited on a silicon semiconductor, quartz semiconductor, or a silicon dioxide semiconductor.

### Claim 27 (depends on 1)

The process to claim 1, wherein the first electrode is deposited on a substrate selected from the group consisting of metal oxide, preferably a transition metal oxide, a metal, a dielectric, paper, a wafer, or a polymeric material.

### Claim 28 (depends on 27)

The process to claim 27, wherein the polymeric material is selected from the group consisting of polyethylene (PE), polypropylene (PP), polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polyimide, polyether ether ketone (PEEK) and polyamide.