# US 10,479,722 B2 · Process for producing structured coatings

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- Number: US 10,479,722 B2
- Document ID: US10479722B2
- Status: Granted
- Kind: B2
- Application number: 15/510,393
- Filed: 2015-09-01
- Published: 2017-10-26
- Granted: 2019-11-19
- Earliest claimed: 2014-09-12
- Assignees: Evonik Degussa GmbH
- Applicants: Evonik Degussa GmbH
- Inventors: Ralf Anselmann; Christian Brinkmoeller; Arne Hoppe; Sonja Merkulov; Gerhard Renner
- Web page: https://patentgrep.com/patent/US10479722B2

## CPC

- C03C 17/007: {containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase}
- C09D 7/61: inorganic
- C09D 183/04: Polysiloxanes
- C23C 18/1212: {Zeolites, glasses}
- C23C 18/122: {Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes}
- C23C 18/1254: {Sol or sol-gel processing}
- C23C 18/127: {Preformed particles}
- G03F 7/11: having cover layers or intermediate layers, e.g. subbing layers {(G03F7/091 - G03F7/093, B41N3/03 take precedence)}
- G03F 7/162: {Coating on a rotating support, e.g. using a whirler or a spinner}
- G03F 7/168: {Finishing the coated layer, e.g. drying, baking, soaking}
- G03F 7/2004: {characterised by the use of a particular light source, e.g. fluorescent lamps or deep UV light}
- G03F 7/32: Liquid compositions therefor, e.g. developers
- G03F 7/426: {containing organic halogen compounds; containing organic sulfonic acids or salts thereof; containing sulfoxides}
- B05D 1/322: {Removable films used as masks}
- B05D 2203/35: Glass
- C03C 2217/40: Coatings comprising at least one inhomogeneous layer
- C03C 2217/45: Inorganic continuous phases
- C03C 2217/485: Pigments
- C03C 2218/113: by sol-gel processes
- C03C 2218/33: by etching
- C03C 2218/34: Masking
- C08K 3/22: of metals
- C08K 2003/2265: {of iron}
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- 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)
- 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)
- G03F: PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR; (phototypographic composing devices B41B; photosensitive materials or processes for photographic purposes G03C; electrophotography, sensitive layers or processes therefor G03G)
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)

## Abstract

The present invention, relates, to a process, for producing structured coatings, in which a coating composition comprising at least one inorganic binder, at least one oxide pigment which, after addition of a mixture consisting of 15 ml of 1 M oxalic acid and 15 ml of 20% aqueous hydrochloric acid based on 1 g of substance, under standard conditions, leads to a temperature rise of at least 4° C., and at least one solvent is applied to a substrate, the resulting coating composition film is partially coated with a photoresist and the substrate coated with the coating composition and the photoresist is treated with an acid, to the structured layers obtainable by the process and to the use thereof.

## Claims

### Claim 1

A process for producing a structured coating, comprising:
applying
a. a coating composition comprising
i. at least one inorganic binder,
ii. at least one oxide pigment which, after addition of a mixture consisting of 15 ml of 1 M oxalic acid and 15 ml of 20% aqueous hydrochloric acid based on 1 g of substance, under standard conditions, leads to a temperature rise of at least 4° C., and
iii. at least one solvent
to a substrate, to obtain a coating composition film on the substrate,
b. partially coating the resulting coating composition film with a photoresist, and
c. treating the substrate coated with the coating composition film and the photoresist with an acid resulting in a leaching out of said at least one oxide pigment from said coating composition film leaving a leached layer.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the inorganic binder has the generic formula SiaR1bOc(OR2)d with a≥2, b≥0, c≥1, d≥5 and R1 and R2=organic radical.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the pigment is a pigment based on a mixed oxide of a (semi)metal in more than one oxidation state and/or a pigment based on at least two mixed oxides of at least two (semi)metals each in one or more oxidation states.

### Claim 4 (depends on 3)

The process according to claim 3, wherein said pigment is a mixed iron-manganese oxide.

### Claim 5 (depends on 4)

The process according to claim 4, wherein said pigment is a copper-containing mixed iron-manganese oxide.

### Claim 6 (depends on 5)

The process according to claim 5, wherein the mixed iron-manganese oxide is obtainable via a calcination of manganese(II) oxide, manganese(III) oxide, iron(II) oxide and iron(III) oxide and copper(II) oxide.

### Claim 7 (depends on 6)

The process according to claim 6, wherein the pigment is assigned to the group of pigments having the Colour Index designation Pigment Black 26.

### Claim 8 (depends on 1)

The process according to claim 1, wherein a proportion of oxide pigment, based on the total mass of the composition, is 10%-50% by weight.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the at least one solvent is selected from the group consisting of an alcohol, an alkyl ester, an alkoxy alcohol, an alkoxyalkyl ester and mixtures thereof.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the acid used is aqueous oxalic acid in a concentration of 0.3 to 2.5 mol/l, aqueous hydrochloric acid 3.0-12.0 mol/l or mixtures having proportion by volume ratios of 1:2 to 2:1 of 1 M aqueous oxalic acid and 6 M aqueous HCl.

### Claim 11 (depends on 1)

The process according to claim 1, wherein after the acid treatment
a. the photoresist is removed, and
b. the coating composition is cured.

### Claim 12 (depends on 1)

The process according to claim 1, wherein after the acid treatment
a. a portion of said coating composition film which is not coated with said photoresist is removed partially or completely,
b. the photoresist is removed, and
c. the coating composition is cured.

### Claim 13 (depends on 1)

The process according to claim 1, wherein as a result of acid treatment portions of said coating composition film exposed to acid becomes transparent.

### Claim 14 (depends on 1)

The process according to claim 1, wherein as a result of acid treatment, portions of said coating composition film exposed to acid become free of oxide pigment.

### Claim 15 (depends on 1)

The process according to claim 1, wherein as a result of acid treatment portions of said coating composition film exposed to acid are not etched.