EP3342900A1 - Composition for cleaning and inhibition of build-ups in coating nozzles for solution process metal oxide precursors - Google Patents

Composition for cleaning and inhibition of build-ups in coating nozzles for solution process metal oxide precursors Download PDF

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Publication number
EP3342900A1
EP3342900A1 EP16206963.7A EP16206963A EP3342900A1 EP 3342900 A1 EP3342900 A1 EP 3342900A1 EP 16206963 A EP16206963 A EP 16206963A EP 3342900 A1 EP3342900 A1 EP 3342900A1
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EP
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Prior art keywords
metal
alkoxides
combinations
acetylacetone
coating
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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EP16206963.7A
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German (de)
French (fr)
Inventor
Dennis Weber
Alexey Merkulov
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Evonik Operations GmbH
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Evonik Degussa GmbH
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Priority to EP16206963.7A priority Critical patent/EP3342900A1/en
Priority to PCT/EP2017/084174 priority patent/WO2018122110A1/en
Priority to TW106145268A priority patent/TW201842177A/en
Publication of EP3342900A1 publication Critical patent/EP3342900A1/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/26—Processes for applying liquids or other fluent materials performed by applying the liquid or other fluent material from an outlet device in contact with, or almost in contact with, the surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
    • B05D2401/10—Organic solvent

Definitions

  • the present invention relates to a nozzle coating method for depositing metal alkoxides and / or metal oxo alkoxides, wherein the nozzle is immersed in a solvent before and / or after the coating process.
  • the present invention also relates to the use of a solvent for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles. It also relates to the use of a solvent for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles.
  • Slot die coating is a coating technique used to apply thin layers of liquid to web-like substrates (paper, foil, fabrics, etc.) or piece goods (glass, metal plates, etc.).
  • substrates in the coating industry especially for those with functional layers (photovoltaics, medical products, wafers, lithium-ion batteries, fuel cells, etc.)
  • the accuracy of the layer thicknesses to be applied is of essential importance. Uncontrollable layer thickness variations due to changes in production conditions or changes in fluid properties are not acceptable for a variety of coatings.
  • defect-free coatings of substrates not only require reliable and easy-to-use processes and application tools, such as the nozzles, but also make special demands on the coating fluids used, eg. B. their freedom from bubbles.
  • controlled stirring processes are required to ensure consistent properties of the applied coating fluids for defect-free layers on substrates.
  • the fluid supply to the coating tools used must be pulsation-free in order to produce flawless films on substrates. It is thus the reproducible, controlled interaction of all the products and peripheral processes of a coating process that must be mastered to achieve film layers on high quality substrates, as in US Pat FIG. 1 shown.
  • Coating fluids are solutions of one or more solids in a solvent. Between the individual coating operations, the nozzle is immersed in a trough with a solvent to prevent drying of the solid contained in the coating fluid.
  • the composition of the solvent in the tub corresponds to the composition of the solvent in the coating fluid, or only the component is involved in the tub submitted the highest volume fraction in the solvent of the coating fluid.
  • the process of this process is schematic in FIG. 2 shown.
  • Coating fluids containing metal oxide precursors may tend to sol-gel reaction. It is mainly in the interior of the nozzle, which is usually made of stainless steel, deposits of the solid on the die lips. The deposits do not re-dissolve during the coating process and can not be removed by rinsing with the solvent of the coating fluid.
  • Metal oxide precursors which tend to sol-gel in solution are organometallic compounds such as metal alkoxides and metal oxo alkoxides.
  • the object of the present invention was therefore to provide a nozzle coating method for depositing metal alkoxides and / or metal oxo alkoxides, which overcomes the disadvantages of the prior art.
  • a nozzle coating method for the deposition of metal alkoxides and / or metal oxo-alkoxides characterized in that the nozzle before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone is immersed ,
  • acetylacetone prevents the sol-gel reaction by chelating the organometallic precursor, or makes deposits that have become soluble again by complexation.
  • the inventive method is not limited to a particular nozzle shape, but is suitable for all geometries and types of slot dies, such as slot dies.
  • the solvent contains at least 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 or 95 wt .-% acetylacetone.
  • the solvent contains 100% by weight of acetylacetone, i. the solvent consists of acetylacetone.
  • the metal is selected from the group consisting of indium, zinc, tin, gallium, aluminum, titanium, hafnium, yttrium or combinations thereof.
  • the inventive method z.
  • metal alkoxides titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof.
  • the deposited metal alkoxide and / or metal oxo alkoxide, as described above, is dissolved in a solvent selected from the group consisting of glycol ethers having a, such as. For example, 1-methoxy-2-propanol, or more ether groups, such as.
  • a solvent selected from the group consisting of glycol ethers having a, such as. For example, 1-methoxy-2-propanol, or more ether groups, such as.
  • ether groups such as.
  • triethylene glycol monomethyl ether alcohols, such as. For example, ethanol, tetrahydrofurfuryl alcohol, esters, such as.
  • lactates or acetates in particular ethyl lactate, butyl acetate, aromatics, such as. Toluene, or combinations thereof.
  • the present invention also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles. It also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles.
  • the metal alkoxides and / or metal oxo alkoxides in the two uses of the invention metals selected from the group consisting of indium, zinc, tin, gallium, aluminum, titanium, hafnium, yttrium or combinations thereof, on.
  • the two uses according to the invention as metal alkoxides preferably comprise titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof.
  • the present invention is further illustrated by the following example.
  • the commercially available product iXsenic S ® from Evonik Industries AG is a metal-organic precursor for use in a nozzle coating process, which can undergo a sol-gel reaction. With air humidity, the product reacts irreversibly, thus changing chemically. The material crystallizes out in the nozzle. There it accumulates until it comes to a blockage of the nozzle.
  • nozzle If the nozzle is immersed before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone, no clogging of the nozzle is observed. Existing deposits dissolve again.

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  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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Abstract

Die vorliegende Erfindung betrifft ein Düsen-Beschichtungsverfahren zur Abscheidung von Metall-Alkoxiden und/oder Metall-Oxo-Alkoxiden, dadurch gekennzeichnet, dass die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel enthaltend mindestens 25 Gew.-% Acetylaceton eingetaucht wird.The present invention relates to a nozzle coating method for the deposition of metal alkoxides and / or metal oxo alkoxides, characterized in that the nozzle before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone is immersed.

Die vorliegende Erfindung betrifft auch die Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Prävention von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen. Sie betrifft ebenfalls die Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Auflösung von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen.The present invention also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles. It also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles.

Description

Die vorliegende Erfindung betrifft ein Düsen-Beschichtungsverfahren zur Abscheidung von Metall-Alkoxiden und/oder Metall-Oxo-Alkoxiden, wobei die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel eingetaucht wird.The present invention relates to a nozzle coating method for depositing metal alkoxides and / or metal oxo alkoxides, wherein the nozzle is immersed in a solvent before and / or after the coating process.

Die vorliegende Erfindung betrifft auch die Verwendung eines Lösungsmittels zur Prävention von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen. Sie betrifft ebenfalls die Verwendung eines Lösungsmittels zur Auflösung von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen.The present invention also relates to the use of a solvent for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles. It also relates to the use of a solvent for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles.

Die Schlitzdüsen-Beschichtung (englisch: slot die) ist eine Beschichtungstechnik, um dünne Flüssigkeitsschichten auf bahnförmige Substrate (Papier, Folie, Stoffe etc.) oder Stückgüter (Glas, Metallplatten etc.) aufzutragen. Für einige Substrate in der Beschichtungsindustrie, vor allem für solche mit Funktionsschichten (Fotovoltaik, medizinische Produkte, Wafer, Lithium-Ionen-Batterien, Brennstoffzellen etc.), ist die Genauigkeit der aufzutragenden Schichtdicken von essentieller Bedeutung. Unkontrollierbare Schichtdickenvariationen, bedingt durch Änderungen der Produktionsbedingungen oder durch Änderungen der Fluideigenschaften, sind hierbei für eine Vielzahl von Beschichtungen nicht vertretbar.Slot die coating is a coating technique used to apply thin layers of liquid to web-like substrates (paper, foil, fabrics, etc.) or piece goods (glass, metal plates, etc.). For some substrates in the coating industry, especially for those with functional layers (photovoltaics, medical products, wafers, lithium-ion batteries, fuel cells, etc.), the accuracy of the layer thicknesses to be applied is of essential importance. Uncontrollable layer thickness variations due to changes in production conditions or changes in fluid properties are not acceptable for a variety of coatings.

Fehlerfreie Beschichtungen von Substraten erfordern aber nicht nur verlässlich arbeitende und leicht bedienbare Prozesse und Auftragswerkzeuge, wie beispielsweise die Düsen, sondern stellen darüber hinaus auch besondere Anforderungen an die eingesetzten Beschichtungsfluide, z. B. deren Blasenfreiheit. Oftmals sind kontrollierte Rührprozesse erforderlich, um konstante Eigenschaften der angesetzten Beschichtungsfluide für fehlerfreie Schichten auf Substraten sicherzustellen. Hinzu kommt, dass die Fluidzuführung zu den eingesetzten Beschichtungswerkzeugen pulsationsfrei erfolgen muss, um fehlerfreie Filme auf Substraten zu erzeugen. Es ist somit das reproduzierbare, kontrollierte Zusammenwirken aller Produkte und peripheren Prozesse eines Beschichtungsvorgangs, die beherrscht werden müssen, um Filmschichten auf Substraten mit hoher Qualität zu erreichen, wie in Figur 1 dargestellt.However, defect-free coatings of substrates not only require reliable and easy-to-use processes and application tools, such as the nozzles, but also make special demands on the coating fluids used, eg. B. their freedom from bubbles. Often, controlled stirring processes are required to ensure consistent properties of the applied coating fluids for defect-free layers on substrates. In addition, the fluid supply to the coating tools used must be pulsation-free in order to produce flawless films on substrates. It is thus the reproducible, controlled interaction of all the products and peripheral processes of a coating process that must be mastered to achieve film layers on high quality substrates, as in US Pat FIG. 1 shown.

Beschichtungsfluide sind Lösungen eines oder mehrerer Feststoffe in einem Lösungsmittel. Zwischen den einzelnen Beschichtungsvorgängen wird die Düse in eine Wanne mit einem Lösungsmittel eingetaucht, um eine Trocknung des im Beschichtungsfluid enthaltenen Feststoffs zu vermeiden. Dabei entspricht die Zusammensetzung des Lösungsmittels in der Wanne der Zusammensetzung des Lösungsmittels in dem Beschichtungsfluid, oder es wird in der Wanne lediglich die Komponente mit dem höchsten Volumenanteil in dem Lösungsmittel des Beschichtungsfluids vorgelegt. Der Ablauf dieses Prozesses ist schematisch in Figur 2 dargestellt.
Beschichtungsfluide enthaltend Metalloxid-Präkursoren können zur Sol-Gel Reaktion neigen. Dabei kommt es vor allem im Inneren der Düse, welche in der Regel aus Edelstahl gefertigt ist, zu Ablagerungen des Feststoffs an den Düsenlippen. Die Ablagerungen lösen sich im Verlauf des Beschichtungsverfahrens nicht wieder auf und können auch durch Spülen mit dem Lösungsmittel des Beschichtungsfluids nicht entfernt werden. Metalloxid-Präkursoren, welche in Lösung zur Sol-Gel Reaktion neigen, sind metallorganische Verbindungen, wie Metall-Alkoxide und Metall-Oxo-Alkoxide.Coating fluids are solutions of one or more solids in a solvent. Between the individual coating operations, the nozzle is immersed in a trough with a solvent to prevent drying of the solid contained in the coating fluid. In this case, the composition of the solvent in the tub corresponds to the composition of the solvent in the coating fluid, or only the component is involved in the tub submitted the highest volume fraction in the solvent of the coating fluid. The process of this process is schematic in FIG. 2 shown.
Coating fluids containing metal oxide precursors may tend to sol-gel reaction. It is mainly in the interior of the nozzle, which is usually made of stainless steel, deposits of the solid on the die lips. The deposits do not re-dissolve during the coating process and can not be removed by rinsing with the solvent of the coating fluid. Metal oxide precursors which tend to sol-gel in solution are organometallic compounds such as metal alkoxides and metal oxo alkoxides.

Aufgabe der vorliegenden Erfindung war es daher, ein Düsen-Beschichtungsverfahren zur Abscheidung von Metall-Alkoxiden und/oder Metall-Oxo-Alkoxiden bereitzustellen, welches die genannten Nachteile des Standes der Technik überwindet.The object of the present invention was therefore to provide a nozzle coating method for depositing metal alkoxides and / or metal oxo alkoxides, which overcomes the disadvantages of the prior art.

Diese Aufgabe wird erfindungsgemäß gelöst durch ein Düsen-Beschichtungsverfahren zur Abscheidung von Metall-Alkoxiden und/oder Metall-Oxo-Alkoxiden dadurch gekennzeichnet, dass die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel enthaltend mindestens 25 Gew.-% Acetylaceton eingetaucht wird.This object is achieved by a nozzle coating method for the deposition of metal alkoxides and / or metal oxo-alkoxides, characterized in that the nozzle before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone is immersed ,

Überraschenderweise wurde gefunden, dass sich an den Düsenlippen keine Ablagerungen bilden, wenn die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel enthaltend mindestens 25 Gew.-% Acetylaceton eingetaucht wird. Dabei kann die Formulierung in der Düse unverändert bleiben. Bereits vorhandene Ablagerungen werden wieder aufgelöst.Surprisingly, it has been found that deposits do not form on the die lips when the die is immersed before and / or after the coating process in a solvent containing at least 25% by weight of acetylacetone. The formulation in the nozzle can remain unchanged. Existing deposits are dissolved again.

Es wird angenommen, dass Acetylaceton die Sol-Gel Reaktion durch Chelatisierung des metallorganischen Präkursors verhindert, bzw. entstandene Ablagerungen durch Komplexierung wieder löslich macht.It is assumed that acetylacetone prevents the sol-gel reaction by chelating the organometallic precursor, or makes deposits that have become soluble again by complexation.

Das erfindungsgemäße Verfahren ist nicht auf eine bestimmte Düsenform beschränkt, sondern eignet sich für sämtliche Geometrien und Typen von Schlitzdüsen, wie beispielsweise Breitschlitzdüsen.The inventive method is not limited to a particular nozzle shape, but is suitable for all geometries and types of slot dies, such as slot dies.

In einer vorteilhaften Ausgestaltung des erfindungsgemäßen Verfahrens enthält das Lösungsmittel mindestens 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 oder 95 Gew.-% Acetylaceton. In einer besonders vorteilhaften Ausgestaltung des erfindungsgemäßen Verfahrens enthält das Lösungsmittel 100 Gew.-% Acetylaceton, d.h. das Lösungsmittel besteht aus Acetylaceton.In an advantageous embodiment of the method according to the invention, the solvent contains at least 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 or 95 wt .-% acetylacetone. In a particularly advantageous embodiment of the method according to the invention, the solvent contains 100% by weight of acetylacetone, i. the solvent consists of acetylacetone.

In einer weiteren vorteilhaften Ausgestaltung des erfindungsgemäßen Verfahrens ist das Metall ausgewählt aus der Gruppe bestehend aus Indium, Zink, Zinn, Gallium, Aluminium, Titan, Hafnium, Yttrium oder Kombinationen hiervon.In a further advantageous embodiment of the method according to the invention, the metal is selected from the group consisting of indium, zinc, tin, gallium, aluminum, titanium, hafnium, yttrium or combinations thereof.

Bevorzugt weist das erfindungsgemäße Verfahren z. B. als Metall-Alkoxide Titan(IV)-ethoxid, Aluminium(III)-isopropoxid, Hafnium(IV)-ethoxid, Yttrium(III)-isopropoxid oder Kombinationen hiervon auf.Preferably, the inventive method z. Example, as metal alkoxides, titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof.

Ebenfalls bevorzugt weist das erfindungsgemäße Verfahren [In6(µ6-O)(µ2-OR)12Cl6]2- mit R = C1-10-Alkylrest, besonders bevorzugt mit R = C2-4-Alkylrest, auf.Also preferably, the inventive method [In 6 ( μ6 -O) ( μ2 -OR) 12 Cl 6 ] 2- with R = C 1-10 alkyl, particularly preferably with R = C 2-4 alkyl radical on.

Es ist erfindungsgemäß bevorzugt, dass das abzuscheidende Metall-Alkoxid und/oder Metall-Oxo-Alkoxid, wie zuvor beschrieben, gelöst ist in einem Lösungsmittel ausgewählt aus der Gruppe bestehend aus Glykolethern mit einer, wie z. B. 1-Methoxy-2-propanol, oder mehreren Ethergruppen, wie z. B. Triethylenglycolmonomethylether, Alkoholen,wie z. B. Ethanol, Tetrahydrofurfurylalkohol, Estern, wie z. B. Lactaten oder Acetaten, insbesondere Ethyllactat, Butylacetat, Aromaten, wie z. B. Toluol, oder Kombinationen hiervon.It is inventively preferred that the deposited metal alkoxide and / or metal oxo alkoxide, as described above, is dissolved in a solvent selected from the group consisting of glycol ethers having a, such as. For example, 1-methoxy-2-propanol, or more ether groups, such as. As triethylene glycol monomethyl ether, alcohols, such as. For example, ethanol, tetrahydrofurfuryl alcohol, esters, such as. As lactates or acetates, in particular ethyl lactate, butyl acetate, aromatics, such as. Toluene, or combinations thereof.

Die vorliegende Erfindung betrifft auch die Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Prävention von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen. Sie betrifft ebenfalls die Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Auflösung von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen.The present invention also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles. It also relates to the use of a solvent containing at least 25 wt .-% acetylacetone for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating nozzles.

Vorteilhafterweise weisen die Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in den beiden erfindungsgemäßen Verwendungen Metalle ausgewählt aus der Gruppe bestehend aus Indium, Zink, Zinn, Gallium, Aluminium, Titan, Hafnium, Yttrium oder Kombinationen hiervon, auf. Bevorzugt weisen die beiden erfindungsgemäßen Verwendungen als Metall-Alkoxide Titan(IV)-ethoxid, Aluminium(III)-isopropoxid, Hafnium(IV)-ethoxid, Yttrium(III)-isopropoxid oder Kombinationen hiervon auf.
Ebenfalls bevorzugt weisen die beiden erfindungsgemäßen Verwendungen [In6(µ6-O)(µ2-OR)12Cl6]2-mit R = C1-10-Alkylrest, besonders bevorzugt mit R = C2-4-Alkylrest, auf.Advantageously, the metal alkoxides and / or metal oxo alkoxides in the two uses of the invention metals selected from the group consisting of indium, zinc, tin, gallium, aluminum, titanium, hafnium, yttrium or combinations thereof, on. The two uses according to the invention as metal alkoxides preferably comprise titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof.
Also preferably, the two uses of the invention [In 6 ( μ6- O) ( μ2 -OR) 12 Cl 6 ] 2- with R = C 1-10 alkyl, particularly preferably with R = C 2-4 alkyl radical, on.

Die vorliegende Erfindung wird durch folgendes Beispiel näher erläutert.The present invention is further illustrated by the following example.

Beispiel:Example:

Bei dem kommerziell erhältlichen Produkt iXsenic S® der Evonik Industries AG handelt es sich um eine metall-organische Vorstufe zur Verwendung in einem Düsen-Beschichtungsverfahren, welche eine Sol-Gel Reaktion eingehen kann. Mit Luftfeuchtigkeit reagiert das Produkt irreversibel, verändert sich somit chemisch. Dabei kristallisiert das Material in der Düse aus. Dort akkumuliert es sich, bis es zu einer Verstopfung der Düse kommt.The commercially available product iXsenic S ® from Evonik Industries AG is a metal-organic precursor for use in a nozzle coating process, which can undergo a sol-gel reaction. With air humidity, the product reacts irreversibly, thus changing chemically. The material crystallizes out in the nozzle. There it accumulates until it comes to a blockage of the nozzle.

Wird die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel enthaltend mindestens 25 Gew.-% Acetylaceton eingetaucht, ist kein Verstopfen der Düse zu beobachten. Bereits vorhandene Ablagerungen lösen sich wieder auf.If the nozzle is immersed before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone, no clogging of the nozzle is observed. Existing deposits dissolve again.

Claims (15)

Düsen-Beschichtungsverfahren zur Abscheidung von Metall-Alkoxiden und/oder Metall-Oxo-Alkoxiden, dadurch gekennzeichnet, dass die Düse vor und/oder nach dem Beschichtungsverfahren in ein Lösungsmittel enthaltend mindestens 25 Gew.-% Acetylaceton eingetaucht wird.A nozzle coating method for the deposition of metal alkoxides and / or metal oxo alkoxides, characterized in that the nozzle before and / or after the coating process in a solvent containing at least 25 wt .-% acetylacetone is immersed. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Düse ausgewählt ist unter Schlitzdüsen, vorzugsweise eine Breitschlitzdüse ist.A method according to claim 1, characterized in that the nozzle is selected from slot dies, preferably a slot die. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das Lösungsmittel mindestens 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 oder 95 Gew.-% Acetylaceton enthält.A method according to claim 1 or 2, characterized in that the solvent contains at least 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 or 95 wt .-% acetylacetone. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das Lösungsmittel aus Acetylaceton besteht.A method according to claim 1 or 2, characterized in that the solvent consists of acetylacetone. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass das Metall ausgewählt ist aus der Gruppe bestehend aus Indium, Zink, Zinn, Gallium, Aluminium, Titan, Hafnium, Yttrium oder Kombinationen hiervon.Method according to one of claims 1 to 4, characterized in that the metal is selected from the group consisting of indium, zinc, tin, gallium, aluminum, titanium, hafnium, yttrium or combinations thereof. Verfahren nach Anspruche 5, dadurch gekennzeichnet, dass das Metall-Alkoxid ausgewählt ist aus der Gruppe bestehend aus Titan(IV)-ethoxid, Aluminium(III)-isopropoxid, Hafnium(IV)-ethoxid, Yttrium(III)-isopropoxid oder Kombinationen hiervon.A method according to claim 5, characterized in that the metal alkoxide is selected from the group consisting of titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof , Verfahren nach Anspruch 5, dadurch gekennzeichnet, dass es [In6(µ6-O)(µ2-OR)12Cl6]2- mit R = C1-10-Alkylrest, besonders bevorzugt mit R = C2-4-Alkylrest, aufweist.A method according to claim 5, characterized in that it [In 6 ( μ6- O) ( μ2 -OR) 12 Cl 6 ] 2- with R = C 1-10 alkyl, particularly preferably with R = C 2-4 alkyl , having. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass das Metall-Alkoxid und/oder Metall-Oxo-Alkoxid gelöst ist in einem Lösungsmittel ausgewählt aus der Gruppe bestehend aus Glykolethern mit einer oder mehreren Ethergruppen, Alkoholen, Estern, Aromaten oder Kombinationen hiervon.Method according to one of claims 1 to 7, characterized in that the metal alkoxide and / or metal oxo alkoxide is dissolved in a solvent selected from the group consisting of glycol ethers having one or more ether groups, alcohols, esters, aromatics or combinations hereof. Verfahren nach Anspruch 8, dadurch gekennzeichnet, dass die Glykolether mit einer oder mehreren Ethergruppen 1-Methoxy-2-propanol oder Triethylenglycolmonomethylether aufweisen, die Alkohole Ethanol, oder Tetrahydrofurfurylalkohol aufweisen, die Ester Ethyllactat oder Butylacetat aufweisen, die Aromaten Toluol aufweisen oder Kombinationen hiervon.A method according to claim 8, characterized in that the glycol ethers having one or more ether groups 1-methoxy-2-propanol or triethylene glycol monomethyl ether, the alcohols ethanol, or tetrahydrofurfuryl have, the esters ethyl lactate or butyl acetate having aromatics toluene or combinations thereof. Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Prävention von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen, dadurch gekennzeichnet, dass die Metalle ausgewählt sind aus der Gruppe bestehend aus Indium, Zink, Zinn, Gallium, Aluminium, Titan, Hafnium, Yttrium oder Kombinationen hiervon.Use of a solvent containing at least 25 wt .-% acetylacetone for the prevention of deposits by metal alkoxides and / or metal oxo alkoxides in coating dies, characterized in that the metals are selected from the group consisting of indium, zinc, tin, gallium , Aluminum, titanium, hafnium, yttrium or combinations thereof. Verwendung nach Anspruch 10, dadurch gekennzeichnet, dass sie als Metall-Alkoxide Titan(IV)-ethoxid, Aluminium(III)-isopropoxid, Hafnium(IV)-ethoxid, Yttrium(III)-isopropoxid oder Kombinationen hiervon aufweist.Use according to claim 10, characterized in that it comprises, as metal alkoxides, titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof. Verwendung nach Anspruch 10, dadurch gekennzeichnet, dass es [In6(µ6-O)(µ2-OR)12Cl6]2-mit R = C1-10-Alkylrest, besonders bevorzugt mit R = C2-4-Alkylrest, aufweist.Use according to Claim 10, characterized in that it contains [In 6 ( μ 6 -O) ( μ 2 -OR) 12 Cl 6 ] 2- with R = C 1-10 -alkyl, particularly preferably with R = C 2-4 -alkyl , having. Verwendung eines Lösungsmittels enthaltend mindestens 25 Gew.-% Acetylaceton zur Auflösung von Ablagerungen durch Metall-Alkoxide und/oder Metall-Oxo-Alkoxide in Beschichtungsdüsen, dadurch gekennzeichnet, dass die Metalle ausgewählt sind aus der Gruppe bestehend aus Indium, Zink, Zinn, Gallium, Aluminium, Titan, Hafnium, Yttrium oder Kombinationen hiervon.Use of a solvent containing at least 25 wt .-% acetylacetone for the dissolution of deposits by metal alkoxides and / or metal oxo alkoxides in coating dies, characterized in that the metals are selected from the group consisting of indium, zinc, tin, gallium , Aluminum, titanium, hafnium, yttrium or combinations thereof. Verwendung nach Anspruch 13, dadurch gekennzeichnet, dass sie als Metall-Alkoxide Titan(IV)-ethoxid, Aluminium(III)-isopropoxid, Hafnium(IV)-ethoxid, Yttrium(III)-isopropoxid oder Kombinationen hiervon aufweist.Use according to claim 13, characterized in that it comprises, as metal alkoxides, titanium (IV) ethoxide, aluminum (III) isopropoxide, hafnium (IV) ethoxide, yttrium (III) isopropoxide or combinations thereof. Verwendung nach Anspruch 13, dadurch gekennzeichnet, dass es [In6(µ6-O)(µ2-OR)12Cl6]2-mit R = C1-10-Alkylrest, besonders bevorzugt mit R = C2-4-Alkylrest, aufweist.Use according to claim 13, characterized in that it [In 6 ( μ6 -O) ( μ2 -OR) 12 Cl 6 ] 2- with R = C 1-10 -alkyl radical, particularly preferably with R = C 2-4 -alkyl radical , having.
EP16206963.7A 2016-12-27 2016-12-27 Composition for cleaning and inhibition of build-ups in coating nozzles for solution process metal oxide precursors Withdrawn EP3342900A1 (en)

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EP16206963.7A EP3342900A1 (en) 2016-12-27 2016-12-27 Composition for cleaning and inhibition of build-ups in coating nozzles for solution process metal oxide precursors
PCT/EP2017/084174 WO2018122110A1 (en) 2016-12-27 2017-12-21 Composition for cleaning and preventing deposits in coating nozzles for metal oxide precursors which can be processed in solution
TW106145268A TW201842177A (en) 2016-12-27 2017-12-22 Composition for cleaning and preventing deposits in coating nozzles for solubilizable metal oxide precursors

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JPH07282653A (en) * 1994-04-04 1995-10-27 Mitsubishi Materials Corp Manufacture of transparent conductive film
JP2011083695A (en) * 2009-10-15 2011-04-28 Ricoh Co Ltd Inkjet type image forming apparatus
WO2013186082A2 (en) * 2012-06-13 2013-12-19 Evonik Industries Ag Method for producing indium oxide-containing layers
US20160052013A1 (en) * 2013-03-29 2016-02-25 Ricoh Company, Ltd Curtain coating machine and curtain coating method

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Publication number Priority date Publication date Assignee Title
JPH07282653A (en) * 1994-04-04 1995-10-27 Mitsubishi Materials Corp Manufacture of transparent conductive film
JP2011083695A (en) * 2009-10-15 2011-04-28 Ricoh Co Ltd Inkjet type image forming apparatus
WO2013186082A2 (en) * 2012-06-13 2013-12-19 Evonik Industries Ag Method for producing indium oxide-containing layers
US20160052013A1 (en) * 2013-03-29 2016-02-25 Ricoh Company, Ltd Curtain coating machine and curtain coating method

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