# US 10,502,995 B2 · Dielectric siloxane particle films, and devices having the same

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- Number: US 10,502,995 B2
- Document ID: US10502995B2
- Status: Granted
- Kind: B2
- Application number: 15/319,818
- Filed: 2015-06-22
- Published: 2017-05-11
- Granted: 2019-12-10
- Earliest claimed: 2014-06-19
- Assignees: Inkron Oy
- Applicants: Inkron Oy
- Inventors: Juha Rantala; Jarkko Heikkinen; Janne Kylmä
- Web page: https://patentgrep.com/patent/US10502995B2

## CPC

- G02F 1/133345: {Insulating layers (G02F1/1335, G02F1/1337, G02F1/135, G02F1/136 take precedence)}
- C08G 77/14: containing silicon bound to oxygen-containing groups
- C08G 77/80: {Siloxanes having aromatic substituents, e.g. phenyl side groups}
- C08K 3/22: of metals
- C08K 3/28: Nitrogen-containing compounds
- C08L 83/00: Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L 83/06: containing silicon bound to oxygen-containing groups (C08L83/12 takes precedence)
- C09D 5/00: Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced {(electrically insulating plastics, resins or waxes H01B3/30)}; Filling pastes
- C09D 7/61: inorganic
- C09D 7/67: {Particle size smaller than 100 nm}
- C09D 183/06: containing silicon bound to oxygen-containing groups (C09D183/12 takes precedence)
- C09J 7/30: characterised by the adhesive composition
- C09J 9/00: Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks (C09J7/00 takes precedence)
- C09J 11/04: inorganic
- G02F 1/13338: {Input devices, e.g. touch panels}
- G06F 3/0445: {using two or more layers of sensing electrodes, e.g. using two layers of electrodes separated by a dielectric layer}
- G06F 3/0446: {using a grid-like structure of electrodes in at least two directions, e.g. using row and column electrodes}
- H10H 20/854: characterised by their material, e.g. epoxy or silicone resins
- H10K 59/40: OLEDs integrated with touch screens
- C08G 77/18: to alkoxy or aryloxy groups
- C08G 77/20: containing silicon bound to unsaturated aliphatic groups
- C08G 77/62: Nitrogen atoms
- C08K 2003/2244: {of zirconium}
- C08K 2201/003: Additives being defined by their diameter
- C08K 2201/005: Additives being defined by their particle size in general
- C09J 183/06: containing silicon bound to oxygen-containing groups (C09J183/12 takes precedence)
- C09J 2203/318: for the production of liquid crystal displays
- C09J 2301/312: parameters being the characterizing feature
- C09J 2301/408: additives as essential feature of the adhesive layer
- C09J 2467/006: in the substrate
- C09J 2483/00: Presence of polysiloxane
- G02F 2202/023: curable
- G02F 2202/28: Adhesive materials or arrangements
- G02F 2202/36: Micro- or nanomaterials
- G06F 3/0412: {Digitisers structurally integrated in a display}
- H10K 2102/00: Constructional details relating to the organic devices covered by this subclass
- H10K 2102/331: {Nanoparticles used in non-emissive layers, e.g. in packaging layer}
- G02F: OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- 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)
- C09J: ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES (preparation of glue or gelatine C09H)
- G06F: ELECTRIC DIGITAL DATA PROCESSING (computer systems based on specific computational models G06N)
- H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES

## Abstract

A method for making a dielectric film includes a substrate on which is deposited a siloxane starting material and particles, wherein the siloxane starting material has a siloxane polymer, a siloxane oligomer and/or silane monomers, and wherein the particles have an average particle size of less than 400 nm. After deposition, heat and/or electromagnetic energy is applied to the siloxane particle layer so as to cure the layer and form a dielectric film on the substrate. The formed film is optically transmissive to visible light and transmits at least 80% of the visible light incident thereon, and is electrically insulating and has a sheet resistance of 1000 Ω/sq or more.

## Claims

### Claim 1

A dielectric film comprising:
formed on a supporting substrate, a dielectric layer comprising a siloxane polymer and particles within the siloxane polymer and having an average particle size of less than 1 micron;
wherein the dielectric layer is optically transmissive to visible light and transmits at least 75% of the light incident thereon; and
wherein the dielectric layer is electrically insulating and has a sheet resistance of 1000 Ω/sq or more, and
wherein the dielectric film has substantially no —OH groups in the siloxane polymer and has substantially no —H groups directly bonded to Si in the siloxane polymer.

### Claim 2 (depends on 1)

The dielectric film of claim 1, wherein the sheet resistance is 1×105 Ω/sq.

### Claim 3 (depends on 1)

The dielectric film of claim 1, having a refractive index of 1.5 to 2.0.

### Claim 4 (depends on 1)

The dielectric film of claim 1, wherein the particles are ceramic particles.

### Claim 5 (depends on 1)

The dielectric film of claim 1, wherein particles are nanoparticles having an average particle size of 400 nm or less.

### Claim 6 (depends on 4)

The dielectric film of any of claim 4, wherein the particles comprise an oxide of silicon, zinc, aluminum, yttrium, tungsten, titanium-silicon, titanium, antimony, nickel, nickel cobalt, molybdenum, magnesium, manganese, any lanthanide, iron, indium tin, copper, cobalt aluminum, chromium, cesium or calcium; or wherein the particles are aluminum nitride, tantalum nitride, boron nitride, titanium nitride, copper nitride, molybdenum nitride, tungsten nitride, iron nitride, silicon nitride, indium nitride, gallium nitride or carbon nitride.

### Claim 7 (depends on 4)

The dielectric film of claim 4, wherein the particles are nanoparticles having an average particle size of less than 400 nm and wherein the nanoparticles are an oxide of titanium, tantalum, aluminum, zirconium, hafnium or selenium.

### Claim 8 (depends on 1)

The dielectric film of claim 1, wherein the particles are silica, hollow silica, ZrO2, ZrO, TiO2, Ta2O5, antimony tin oxide, or SnO2, which film transmits at least 85% of the visible light incident thereon.

### Claim 9 (depends on 1)

The dielectric film of claim 1, wherein the substrate comprises glass, quartz, sapphire, organic polymer or hybrid organic-inorganic polymer, polyethylene terephthalate, or polymethyl methacrylate.

### Claim 10 (depends on 1)

The dielectric film of claim 1, which is part of a display or part of an OLED device.

### Claim 11 (depends on 1)

The dielectric film of claim 1, wherein the siloxane polymer comprises organic aryl group.

### Claim 12 (depends on 1)

The dielectric film of claim 1, having a refractive index of from 1.6 to 1.9, and wherein the film is thermally stable and if heated to at least 200° C. would have a mass loss of less than 4%.

### Claim 13 (depends on 1)

The dielectric film of claim 1, which is an adhesive in a touchscreen display.

### Claim 14

A method for making a dielectric film, comprising:
providing a substrate; and
depositing on the substrate a composition having a siloxane starting material and particles;
wherein the siloxane starting material comprises a siloxane polymer, a siloxane oligomer and/or silane monomers, and
wherein the particles have an average particle size of less than 400 nm;
wherein heat and/or electromagnetic energy is applied to the siloxane particle layer so as to cure the layer and form a dielectric film on the substrate;
wherein the film is optically transmissive to visible light and transmits at least 80% of the visible light incident thereon;
and wherein the film is electrically insulating and has a sheet resistance of 1000 Ω/sq or more, said siloxane starting material being substantially free of hydrogen directly bonded to silicon and substantially free of —OH groups.

### Claim 15 (depends on 14)

The method of claim 14, wherein the siloxane starting material is deposited together with the particles on the substrate in the absence of a solvent, wherein the particles are oxide nanoparticles having an average particle size of less than 200 nm and where the film has a refractive index of from 1.6 to 1.9.

### Claim 16 (depends on 14)

The method of claim 14, wherein the siloxane starting material comprises organic groups selected from aryl and/or alkyl groups bound to Si in the siloxane backbone.

### Claim 17 (depends on 14)

The method of claim 14, wherein a mass loss of the siloxane composition before and after curing is less than 4%.

### Claim 18 (depends on 14)

The method of claim 14, wherein the siloxane starting material is a photo-crosslinkable polymer, and wherein the siloxane starting material comprises a siloxane polymer, a silane monomer, and an additive, and wherein the additive comprises a reducing agent, a surfactant, a stabilizer, an adhesion promoter, and/or an antioxidant.

### Claim 19 (depends on 14)

The method of claim 14, wherein the siloxane starting material on the substrate is exposed to ultraviolet (UV) light via a mask or patterned photoresist layer, so as to form hardened areas exposed to the UV light surrounded by softer areas in the non-exposed areas, followed by selectively removing the non-exposed areas to form a patterned dielectric film.

### Claim 20 (depends on 14)

The method of claim 14, wherein the particles comprise an oxide of silicon, zinc, aluminum, yttrium, ytterbium, tungsten, titanium-silicon, titanium, antimony, samarium, nickel, nickel cobalt, molybdenum, magnesium, manganese, lanthanide, iron, indium tin, copper, cobalt aluminum, chromium, cesium or calcium, wherein the refractive index of the film is from 1.6 to 1.9, and wherein the particles have an average particle size of less than 50 nm.

### Claim 21 (depends on 14)

The method of claim 14, wherein the siloxane starting material comprises phenyl and a methacrylate functional reactive group, and wherein the particles are ceramic oxide nanoparticles and have an average particle size of less than 400 nm.

### Claim 22 (depends on 14)

The method of claim 14, wherein the siloxane starting material is soft baked, followed by selective exposure to ultraviolet light, followed by removal of selected areas with a developer.

### Claim 23 (depends on 14)

The method of claim 14, wherein the siloxane starting material is heat cured at a temperature of less than 120° C.

### Claim 24 (depends on 14)

The method of claim 14, wherein the siloxane starting material is heat cured at a temperature of less than 125° C. and cured with ultraviolet light; or wherein the siloxane starting material is heat cured at a temperature of less than 100° C. and without the application of ultraviolet light.

### Claim 25 (depends on 14)

The method of claim 14, wherein the siloxane starting material comprises functional cross-linking groups that are independently alkene, alkyne, epoxy, oxetane, or acrylate groups.

### Claim 26

A display comprising:
a plurality of pixels in a matrix, the pixels each comprising a liquid crystal layer and/or light emitting diode layer,
a plurality of substrates that are optically transmissive to visible light;
an adhesive layer for bonding a first substrate to a second substrate and being formed from an electrically insulating material that has a sheet resistance of more than 1000 Ω/sq and that comprises a siloxane material and particles having an average particle size of less than 400 nm,
and, wherein the electrically insulating material is thermally stable where if heated to at least 200° C. the electrically insulating material has a mass loss of less than 2%.

### Claim 27 (depends on 26)

The display of claim 26, wherein the electrically insulating material is an optically transmissive layer that transmits at least 85% of the visible light incident thereon, and wherein the electrically insulating material has a sheet resistance of 10000 Ω/sq.

### Claim 28 (depends on 26)

The display of claim 26, wherein the particles are nitride particles selected from aluminum nitride, tantalum nitride, boron nitride, titanium nitride, copper nitride, molybdenum nitride, tungsten nitride, iron nitride, silicon nitride, indium nitride, gallium nitride or carbon nitride, or the particles are oxide nanoparticles comprising an oxide of silicon, zinc, aluminum, yttrium, ytterbium, tungsten, titanium-silicon, titanium, antimony, samarium, nickel, nickel cobalt, molybdenum, magnesium, manganese, lanthanide, iron, indium tin, copper, cobalt aluminum, chromium, cesium or calcium.

### Claim 29 (depends on 26)

The display of claim 26, wherein the particles comprise an oxide of titanium, tantalum, aluminum, zirconium, hafnium or selenium, and a refractive index of the electrically insulating material is from 1.6 to 1.9.

### Claim 30 (depends on 26)

The display of claim 26, wherein the siloxane material is a siloxane polymer that comprises aryl or alkyl groups and wherein the particles comprise a transition metal oxide, and have an average particle size of less than 100 nm.

### Claim 31 (depends on 26)

The display of claim 26, wherein the plurality of substrates comprise a first substrate having liquid crystal elements thereon, a second substrate comprising a capacitive touch sensor thereon, and a third substrate that is a cover substrate wherein the pixels are twisted nematic liquid crystals.

### Claim 32 (depends on 26)

The display of claim 26, further comprising a second adhesive layer and a third substrate, wherein the second adhesive layers bonds the second and third substrates together.

### Claim 33 (depends on 26)

The display of claim 26, wherein the pixels are light emitting diode (LED) pixels and the first substrate is a flexible polymeric substrate and the display is an OLED display.

### Claim 34 (depends on 26)

The display of claim 26, which is a touch panel display.

### Claim 35

A method for making a display comprising,
providing a first substrate having an array of pixel elements thereon, wherein the pixel elements each comprise a liquid crystal material and/or light emitting diode material;
providing a second substrate that is a cover substrate; and
adhering the first and second substrates together with an adhesive;
wherein the adhesive is comprised of an electrically insulating material that has an electrical resistivity of more than 1000 Ω/sq and that comprises a siloxane material and particles having an average particle size of less than 400 nm;
wherein the first and second substrates are bonded together by applying heat and/or ultraviolet light so as to cure and harden the siloxane material therebetween,
wherein the siloxane material is substantially free of —OH groups, and substantially free of Si—H bonds.

### Claim 36 (depends on 35)

The method of claim 35, wherein the curing is under the application of ultraviolet light, or the curing is under the application of heat at from 120° C. to 150° C.

### Claim 37 (depends on 35)

The method of claim 35, wherein the curing comprises soft baking the siloxane particle material, UV patterning the siloxane particle material, and selectively removing portions of the siloxane particle material so as to leave an electrically insulating pattern, the curing comprises UV patterning the siloxane particle material by the application of UV light via a mask or resist layer.

### Claim 38 (depends on 35)

The method of claim 35, which is a roll-to-roll process and wherein the first substrate is a flexible substrate provided from a roll.

### Claim 39 (depends on 35)

The method of claim 35, wherein the second substrate is a flexible substrate provided from a second roll and for bonding to the first substrate, and wherein the first and second substrates are transparent polymeric materials.

### Claim 40 (depends on 35)

The method of claim 35, wherein the siloxane material comprises aryl groups, and wherein the aryl groups are phenyl groups directly bound to silicon in the siloxane material.