[go: up one dir, main page]

DE102008025108A1 - Process for the production of nanoscale electrically conductive multilayer systems - Google Patents

Process for the production of nanoscale electrically conductive multilayer systems Download PDF

Info

Publication number
DE102008025108A1
DE102008025108A1 DE200810025108 DE102008025108A DE102008025108A1 DE 102008025108 A1 DE102008025108 A1 DE 102008025108A1 DE 200810025108 DE200810025108 DE 200810025108 DE 102008025108 A DE102008025108 A DE 102008025108A DE 102008025108 A1 DE102008025108 A1 DE 102008025108A1
Authority
DE
Germany
Prior art keywords
layer
electrically conductive
oxide
substrate
production
Prior art date
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.)
Granted
Application number
DE200810025108
Other languages
German (de)
Other versions
DE102008025108B4 (en
Inventor
Andreas Dr. Heft
Thomas Struppert
Bernd Dr. Grünler
Andreas Dr. Pfuch
Alexander Jacob
Heinrich Prof. Dr. Lang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
VER ZUR FOERDERUNG VON INNOVAT
Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev)
Original Assignee
VER ZUR FOERDERUNG VON INNOVAT
Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev)
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by VER ZUR FOERDERUNG VON INNOVAT, Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev) filed Critical VER ZUR FOERDERUNG VON INNOVAT
Priority to DE200810025108 priority Critical patent/DE102008025108B4/en
Priority to EP09749502A priority patent/EP2283168A1/en
Priority to PCT/DE2009/050025 priority patent/WO2009140961A1/en
Publication of DE102008025108A1 publication Critical patent/DE102008025108A1/en
Application granted granted Critical
Publication of DE102008025108B4 publication Critical patent/DE102008025108B4/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/453Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating passing the reaction gases through burners or torches, e.g. atmospheric pressure CVD
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3644Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3649Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3655Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating containing at least one conducting layer
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3657Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
    • C03C17/366Low-emissivity or solar control coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3668Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties
    • C03C17/3673Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties specially adapted for use in heating devices for rear window of vehicles
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3681Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating being used in glazing, e.g. windows or windscreens
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/18Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40Oxides
    • C23C16/405Oxides of refractory metals or yttrium
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/78Coatings specially designed to be durable, e.g. scratch-resistant

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Inorganic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

Die Erfindung betrifft ein Verfahren zur Herstellung von nanoskaligen elektrisch leitfähigen Mehrschichtsystemen auf Oberflächen, wobei die beschichteten Oberflächen insbesondere zum Wärme- oder Sonnenschutz bzw. in Heizelementen zur Anwendung kommen. Der Erfindung liegt die Aufgabe zugrunde, eine Möglichkeit anzugeben, welches die genannten Nachteile der etablierten Verfahren zur Abscheidung von elektrisch leitenden Schichten überwindet. Erfindungsgemäß wird diese Aufgabe bei einem Verfahren zum Beschichten von Stubstraten mit einem elektrisch leitenden Schichtsystem dadurch gelöst, dass mindestens eine elektrisch leitende Schicht durch ein Flammenpyrolyse-Verfahren aufgebracht wird.The invention relates to a method for producing nanoscale electrically conductive multilayer systems on surfaces, wherein the coated surfaces are used in particular for heat or sun protection or in heating elements. The invention has for its object to provide a way that overcomes the disadvantages of the established methods for the deposition of electrically conductive layers. According to the invention, this object is achieved in a method for coating substrates with an electrically conductive layer system in that at least one electrically conductive layer is applied by a flame pyrolysis method.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung von nanoskaligen elektrisch leitfähigen Mehrschichtsystemen auf Oberflächen, wobei die beschichteten Oberflächen insbesondere zum Wärme- oder Sonnenschutz bzw. in Heizelementen zur Anwendung kommen.The The invention relates to a method for the production of nanoscale electrically conductive multilayer systems on surfaces, the coated surfaces being used in particular for heat or sunscreen or in heating elements are used.

PVD-Verfahren (Physical vapor deposition) sind seit langem Stand der Technik. Durch Beschuss von Atomen eines Materials mit hochenergetischen Edelgasionen (Sputter-Prozess) ist es möglich, diese aus dem Verbund herauszureißen und auf dem Substrat abzuscheiden.PVD (Physical vapor deposition) have long been state of the art. By bombarding atoms of a material with high energy Inert gas ions (sputtering process) make it possible for these tear out the composite and deposit it on the substrate.

Zum Abscheiden von Metallschichten werden vorwiegend diese PVD-Verfahren (z. B. DE 10 2004 001 655 A1 ) eingesetzt. Diese benötigen jedoch einen sehr aufwendigen und zugleich sehr kostenintensiven Apparaturaufbau, da sehr niedrige Drücke und/oder spezielle Atmosphären benötigt werden.For deposition of metal layers predominantly these PVD methods (eg. DE 10 2004 001 655 A1 ) used. However, these require a very complex and at the same time very expensive equipment construction, since very low pressures and / or special atmospheres are needed.

Bekannt sind auch Verfahren, bei denen in eine Flamme metallorganische und/oder metallanorganische Verbindungen (Precursor) eingebracht und durch Verbrennungsprozesse zersetzt und auf einer Oberfläche abgeschieden wurden. Diese Verfahren werden als Combustion-CVD-Verfahren oder Flammenpyrolyseverfahren bezeichnet. In der Patentanmeldung DE 10 2006 029 617 A1 werden mittels dieses Verfahrens heiße Glasoberflächen beschichtet.Methods are also known in which organometallic and / or organometallic compounds (precursors) are introduced into a flame and decomposed by combustion processes and deposited on a surface. These processes are referred to as combustion CVD processes or flame pyrolysis processes. In the patent application DE 10 2006 029 617 A1 hot glass surfaces are coated by this method.

Die thermische CVD benötigt hohe Substrattemperaturen und ist somit nur für wenige Materialen geeignet. (Lit.: H. J. Gläser, Dünnfilmtechnologie auf Flachglas, Schorndorf, Verlag Karl Hofman, 1999 )The thermal CVD requires high substrate temperatures and is therefore only suitable for a few materials. (Lit .: HJ glasses, thin-film technology on flat glass, Schorndorf, Verlag Karl Hofman, 1999 )

Ebenfalls sind aus der Patentanmeldung DE 43 20 931 A1 Beschichtungen mit elektrisch leitenden Schichten bekannt. Hierbei sind die Mehrschichtsysteme aus haftvermittelnden Schichten, Barriereschichten und Schutzschichten aufgebaut, zwischen denen die elektrisch leitende Schicht angeordnet ist.Also are from the patent application DE 43 20 931 A1 Coatings with electrically conductive layers known. Here, the multilayer systems of adhesion-promoting layers, barrier layers and protective layers are constructed, between which the electrically conductive layer is arranged.

Der Erfindung liegt die Aufgabe zugrunde, eine Möglichkeit anzugeben, welches die genannten Nachteile der etablierten Verfahren zur Abscheidung von elektrisch leitenden Schichten überwindet.Of the Invention is based on the object, a possibility indicate the disadvantages of the established methods for the deposition of electrically conductive layers overcomes.

Erfindungsgemäß wird diese Aufgabe bei einem Verfahren zum Beschichten von Substraten mit einem elektrisch leitenden Schichtsystem dadurch gelöst, dass mindestens eine elektrisch leitende Schicht durch ein Flammenpyrolyse-Verfahren aufgebracht wird. Der wesentliche Vorteil der Erfindung besteht in der verhältnismäßig einfachen und vor allem preiswerten Bauweise des Beschichtungsapparates. Das verwendete Combustion-CVD-Verfahren wird unter Atmosphärendruck und ohne Schutzgase betrieben. Ein weiterer Vorteil der Erfindung besteht in der Verwendung eines relativ kalten Substrates (maximal 80°C Vorwärmtemperatur) wodurch auch thermisch nicht hoch belastbare Materialen, wie Kunststoffe, beschichtet werden können. Zudem wird der Einsatz und die Kombination spezieller Precursoren benötigt, um die gewünschte Eigenschaft des Mehrschichtsystems zu erhalten.According to the invention this task in a process for coating substrates solved with an electrically conductive layer system thereby that at least one electrically conductive layer by a flame pyrolysis method is applied. The main advantage of the invention is in the relatively simple and especially inexpensive construction of the coating apparatus. The used Combustion-CVD method is under atmospheric pressure and operated without shielding gases. Another advantage of the invention is in the use of a relatively cold substrate (maximum 80 ° C Preheating temperature) which also thermally not highly resilient Materials, such as plastics, can be coated. In addition, the use and the combination of special precursors needed to get the desired property of the multilayer system to obtain.

Erfindungsgemäß setzt sich das Mehrschichtsystem aus einzelnen Schichten zusammen, welche verschiedene Zwecke erfüllen. Dazu gehören Haftvermittlung, Barrierewirkung und Schutz. Zwischen diesen einzelnen Schichten wird mindestens eine elektrisch leitende Schicht, welche elementar oder oxidisch sein kann, eingebaut. Das Mehrschichtsystem kann ebenfalls aus mehreren solchen Basisbaugruppen aufgebaut sein. Die Gesamtschichtdicke des Mehrschichtsystems soll unter 200 nm betragen, wobei die Schichtdicken der einzelnen Schichten 10 bis 50 nm betragen.According to the invention sets The multi-layer system of individual layers together, which fulfill different purposes. These include Barrier effect and protection. Between these individual layers is at least one electrically conductive layer, which elemental or oxidic can be incorporated. The multi-layer system can also be composed of several such basic modules. The total layer thickness of the multilayer system should be less than 200 nm, the layer thicknesses the individual layers are 10 to 50 nm.

Die elektrisch leitenden Schichten bestehen aus Silber oder Gold, welche ab einer Schichtdicke von wenigen Nanometer (< 10 nm) eine gute elektrische Leitfähigkeit besitzen und damit für Anwendungen, bei denen eine hohe IR-Reflexion von Bedeutung ist, in Betracht kommen. Silberschichten bieten darüber hinaus bis zu einer bestimmten Schichtdicke (bis ca. 20 nm) eine hohe Transmission im UV- und sichtbaren Bereich.The electrically conductive layers are made of silver or gold, which from a layer thickness of a few nanometers (<10 nm) a good electrical conductivity own and thus for applications where a high IR reflection is important to consider. silver layers also offer up to a certain layer thickness (up to about 20 nm) a high transmission in the UV and visible range.

Erfindungsgemäß ist eine derartige Abscheidung auch mit einem Atmosphärendruck-Plasma denkbar. Die Schichtbildungsprozesse bei der Umwandlung der entsprechenden Precursoren sind denen in der Flamme sehr ähnlich, so dass auch damit elektrisch leitende nanoskalige Mehrschichtsysteme abgeschieden werden können.According to the invention such deposition also with an atmospheric pressure plasma conceivable. The film formation processes in the conversion of the corresponding Precursors are very similar to those in the flame, so that also used to deposit electrically conductive nanoscale multilayer systems can be.

Die Erfindung soll nachstehend anhand von Ausführungsbeispielen näher erläutert werden. In der dazugehörigen Zeichnung zeigtThe Invention will be described below with reference to embodiments be explained in more detail. In the corresponding Drawing shows

1 den Aufbau eines Mehrschichtsystems. 1 the construction of a multi-layer system.

Das erfindungsgemäße Verfahren ist gerichtet auf die Herstellung eines Mehrschichtsystems 1 basierend auf Wolframoxid 3, Zirkonoxid 4, elektrisch leitende Schicht (Silber, Gold, ...) 5 und einer Schutzschicht 6 auf einem Substrat 2. Substrate 2 können dabei Glas, Kunststoff oder sogar Metalle sein.The inventive method is directed to the production of a multi-layer system 1 based on tungsten oxide 3 , Zirconium oxide 4 , electrically conductive layer (silver, gold, ...) 5 and a protective layer 6 on a substrate 2 , substrates 2 can be glass, plastic or even metals.

Beispiel 1example 1

Die Abscheidung eines Mehrschichtsystems 1 auf Glas kann als Wärmeschutzverglasung Anwendung finden. Die elektrisch leitende Schicht, welche vorrangig aber nicht zwangsläufig aus Silber besteht, trägt dabei die Eigenschaft der Reflexion der IR-Strahlung. Silber weist bei einer guten IR-Reflexion noch eine hohe Transmission im UV- und sichtbaren Bereich auf.The deposition of a multilayer system 1 on glass can be used as heat protection glazing application. The electrically conductive layer, which primarily but not necessarily consists of silver, thereby carries the property of the reflection of the IR radiation. Silver still has a high transmission in the UV and visible range with good IR reflection.

Inhalt der erfindungsgemäßen Lösung ist die Kopplung eines oxidischen Mehrschichtsystems mit einer Silberschicht 5. Diese Silberschicht 5 wird hierbei direkt auf das oxidische Mehrschichtsystem bestehend aus Wolframoxid 3 und Zirkonoxid 4 oder auf ein aus mehreren zusätzlichen Schichten bestehendes Mehrschichtsystem aufgebracht. Mindestens die Silberschicht 5 wird dabei flammenpyrolytisch abgeschieden. Als Precursorsubstanzen werden für die flammenpyrolytische Abscheidung der Metall- und Metalloxidschichten metallorganische und/oder metallanorganische Verbindungen, welche das entsprechende Element enthalten, verwendet. Jedoch ist es von Bedeutung, die einzelnen Precursoren aufeinander abzustimmen, um das gewünschte Mehrschichtsystem mit den gewünschten Eigenschaften zu erhalten.Contents of the solution according to the invention is the coupling of an oxide multilayer system with a silver layer 5 , This silver layer 5 is here directly on the oxide multilayer system consisting of tungsten oxide 3 and zirconia 4 or applied to a multi-layer system consisting of several additional layers. At least the silver layer 5 is deposited by flame pyrolysis. As precursor substances, organometallic and / or organometallic compounds containing the corresponding element are used for the flame pyrolytic deposition of the metal and metal oxide layers. However, it is important to tailor the individual precursors in order to obtain the desired multilayer system with the desired properties.

Nachfolgend wird der Parameterbereich für die flammenpyrolytische Abscheidung der einzelnen Schichten angegeben: Flammenpyrolyse-Anlage mit temperierbaren Verfahrtisch und Brenner Gas-Mischung: Brenngasgemisch (Propan/Luft) Volumenstrom Gas: 1–2 l/min Volumenstrom Luft: 20–50 l/min Brenner: Lochbrenner mit Homogenisatoraufsatz (Breite 220 mm) Vorheiztemperatur Verfahrtisch: 30–80°C Geschwindigkeit Verfahrtisch: 15–100 mm/s Abstand Substrat-Brenner: 4–8 mm Parameterbereich für Wolframoxid-Schichtabscheidung Precursor: Ammonium(meta)-wolframat in Methanol/Wasser (2:1) Precursorkonzentration: 0,01–0,5 mol/l Anzahl an Durchläufen: 5–20 Schichtdicke: bis 30 nm Parameterbereich für Zirkonoxid-Schichtabscheidung Precursor: Zirkon(IV)acetylacetonat in Ethanol/Wasser Precursorkonzentration: 0,05–0,5 mol/l Anzahl an Durchläufen: 5–20 Schichtdicke: bis 20 nm Parameterbereich für Silber-Schichtabscheidung Precursor: Silber(I)-carboxylat in Ethanol/Wasser (2:1) Precursorkonzentration: 0,1–0,2 mol/l Anzahl an Durchläufen: 10–100 Schichtdicke: bis 70 nm The parameter range for the flame pyrolytic deposition of the individual layers is given below: Flame pyrolysis system with temperature-controlled travel table and burner Gas mixture: Fuel gas mixture (propane / air) Volume flow of gas: 1-2 l / min Volume flow air: 20-50 l / min Burner: Hole burner with homogenizer attachment (width 220 mm) Preheating temperature traversing table: 30-80 ° C Speed traversing: 15-100 mm / s Distance substrate burner: 4-8 mm Parameter range for tungsten oxide film deposition precursor: Ammonium (meta) tungstate in methanol / water (2: 1) precursor concentration: 0.01-0.5 mol / l Number of passes: 5-20 Layer thickness: up to 30 nm Parameter range for zirconium oxide layer deposition precursor: Zircon (IV) acetylacetonate in ethanol / water precursor concentration: 0.05-0.5 mol / l Number of passes: 5-20 Layer thickness: up to 20 nm Parameter range for silver layer deposition precursor: Silver (I) carboxylate in ethanol / water (2: 1) precursor concentration: 0.1-0.2 mol / l Number of passes: 10-100 Layer thickness: up to 70 nm

Beispiel 2Example 2

Auch der Einsatz von Gold als elektrisch leitende Schicht ist denkbar. Großtechnisch ist die Goldabscheidung eher unrealistisch, da die enorm hohen Rohstoffpreise eine Massenproduktion verhindern. Jedoch für geringe Stückzahlen und/oder nicht flächige Substrate, bei denen eine hohe IR-Reflexion benötigt wird, kann mit der Flammenpyrolyse dieses Mehrschichtsystem sehr kostengünstig aufgebracht werden.Also The use of gold as an electrically conductive layer is conceivable. On a large scale, the gold separation is rather unrealistic, because the enormously high raw material prices prevent mass production. However, for low quantities and / or not flat substrates where high IR reflection is required can, with the flame pyrolysis this multilayer system very much be applied inexpensively.

Inhalt der erfindungsgemäßen Lösung ist die Kopplung eines oxidischen Mehrschichtsystems mit einer Goldschicht. Diese Goldschicht wird hierbei direkt auf das oxidische Mehrschichtsystem bestehend aus Wolframoxid 3 und Zirkonoxid 4 oder auf ein aus mehreren zusätzlichen Schichten bestehendes Mehrschichtsystem aufgebracht. Mindestens die Goldschicht 5 wird dabei flammenpyrolytisch abgeschieden. Als Precursorsubstanzen werden für die flammenpyrolytische Abscheidung der Metall- und Metalloxidschichten werden metallorganische und/oder metallanorganische Verbindungen, welche das entsprechende Element enthalten, verwendet. Jedoch ist es von Bedeutung, die einzelnen Precursoren aufeinander abzustimmen, um das gewünschte Mehrschichtsystem zu erhaltenContent of the solution according to the invention is the coupling of an oxide multilayer system with a gold layer. This gold layer is here directly on the oxide multilayer system consisting of tungsten oxide 3 and zirconia 4 or applied to a multi-layer system consisting of several additional layers. At least the gold layer 5 is deposited by flame pyrolysis. As precursor substances, organometallic and / or organometallic compounds containing the corresponding element are used for the flame pyrolytic deposition of the metal and metal oxide layers. However, it is important to match the individual precursors to one another in order to obtain the desired multilayer system

ZITATE ENTHALTEN IN DER BESCHREIBUNGQUOTES INCLUDE IN THE DESCRIPTION

Diese Liste der vom Anmelder aufgeführten Dokumente wurde automatisiert erzeugt und ist ausschließlich zur besseren Information des Lesers aufgenommen. Die Liste ist nicht Bestandteil der deutschen Patent- bzw. Gebrauchsmusteranmeldung. Das DPMA übernimmt keinerlei Haftung für etwaige Fehler oder Auslassungen.This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.

Zitierte PatentliteraturCited patent literature

  • - DE 102004001655 A1 [0003] DE 102004001655 A1 [0003]
  • - DE 102006029617 A1 [0004] DE 102006029617 A1 [0004]
  • - DE 4320931 A1 [0006] - DE 4320931 A1 [0006]

Zitierte Nicht-PatentliteraturCited non-patent literature

  • - H. J. Gläser, Dünnfilmtechnologie auf Flachglas, Schorndorf, Verlag Karl Hofman, 1999 [0005] - HJ glasses, thin-film technology on flat glass, Schorndorf, Verlag Karl Hofman, 1999 [0005]

Claims (9)

Verfahren zur Herstellung von nanoskaligen elektrisch leitfähigen Mehrschichtsystemen, welches aus einem Substrat und den darüber liegenden Schichten zur Haftvermittlung, zur Barrierewirkung und zum Schutz besteht, dadurch gekennzeichnet, dass mindestens eine elektrisch leitende Schicht mittels eines Flammenpyrolyse-Prozesses bei Atmosphärendruck abgeschieden wird.A process for the production of nano-scale electrically conductive multi-layer systems, which consists of a substrate and the overlying layers for adhesion, barrier effect and protection, characterized in that at least one electrically conductive layer is deposited by means of a flame pyrolysis process at atmospheric pressure. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die elektrisch leitende Schicht als eine metallische Schicht abgeschieden wird.Method according to claim 1, characterized in that that the electrically conductive layer as a metallic layer is deposited. Verfahren nach Anspruch 1, durch gekennzeichnet, dass zuerst auf das Substrat zur Haftvermittlung eine Schicht aus Wolframoxid aufgebracht wird.Method according to claim 1, characterized by first apply a layer to the adhesion promoter substrate Tungsten oxide is applied. Verfahren nach Anspruch 1, durch gekennzeichnet, dass als zweite Schicht zur Barrierewirkung eine Schicht aus Zirkonoxid aufgebracht wird.Method according to claim 1, characterized by that as a second layer for barrier action, a layer of zirconium oxide is applied. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass auf das Substrat als erstes eine Schicht bestehend aus Molybdänoxid aufgebracht wird.Method according to claim 1, characterized in that that on the substrate first, a layer consisting of molybdenum oxide is applied. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass auf das Substrat als erstes eine Schicht bestehend aus Chromoxid aufgebracht wird.Method according to claim 1, characterized in that that on the substrate, first, a layer consisting of chromium oxide is applied. Verfahren nach Anspruch 1, 2 5 oder 6, dadurch gekennzeichnet, dass auf die erste Schicht eine zweite Schicht bestehend aus Zinnoxid aufgebracht wird.Method according to claim 1, 2 5 or 6, characterized that on the first layer, a second layer consisting of tin oxide is applied. Verfahren nach Anspruch 1, 2 5 oder 6, dadurch gekennzeichnet, dass auf die erste Schicht eine zweite Schicht bestehend aus Titanoxidoxid aufgebracht wird.Method according to claim 1, 2 5 or 6, characterized that on the first layer, a second layer consisting of titanium oxide is applied. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass als abschließende Schicht eine Schutzschicht bestehend aus Al-Oxid, Si-Oxid, Sn-Oxid oder Zn-Oxid aufgebracht wird.Method according to one of the preceding claims, characterized in that as the final layer a protective layer consisting of Al oxide, Si oxide, Sn oxide or Zn oxide is applied.
DE200810025108 2008-05-23 2008-05-23 Process for the production of nanoscale electrically conductive multilayer systems Expired - Fee Related DE102008025108B4 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE200810025108 DE102008025108B4 (en) 2008-05-23 2008-05-23 Process for the production of nanoscale electrically conductive multilayer systems
EP09749502A EP2283168A1 (en) 2008-05-23 2009-05-15 Method for producing nanoscalar electrically conductive multilayer systems
PCT/DE2009/050025 WO2009140961A1 (en) 2008-05-23 2009-05-15 Method for producing nanoscalar electrically conductive multilayer systems

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE200810025108 DE102008025108B4 (en) 2008-05-23 2008-05-23 Process for the production of nanoscale electrically conductive multilayer systems

Publications (2)

Publication Number Publication Date
DE102008025108A1 true DE102008025108A1 (en) 2009-11-26
DE102008025108B4 DE102008025108B4 (en) 2012-02-23

Family

ID=41011866

Family Applications (1)

Application Number Title Priority Date Filing Date
DE200810025108 Expired - Fee Related DE102008025108B4 (en) 2008-05-23 2008-05-23 Process for the production of nanoscale electrically conductive multilayer systems

Country Status (3)

Country Link
EP (1) EP2283168A1 (en)
DE (1) DE102008025108B4 (en)
WO (1) WO2009140961A1 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011076203A1 (en) 2009-12-22 2011-06-30 Rent A Scientist Gmbh Formulation comprising metal nanoparticles
DE102010030301A1 (en) 2010-06-21 2011-12-22 Solayer Gmbh Substrate with superficially structured surface electrode
DE102010024521A1 (en) * 2010-06-21 2011-12-22 Innovent E.V. Method for increasing the translucency of a substrate
DE102012003943A1 (en) 2012-02-24 2013-08-29 Innovent E.V. Technologieentwicklung Preparing antimicrobial nano-layers on substrate material, in the form of e.g. fiber- or yarn materials, comprises surface modifying the substrate material by flame-pyrolysis process, and depositing a thin layer on the substrate material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4320931A1 (en) 1992-10-21 1994-04-28 Solvay Deutschland Deposition of layers with high specific electrical conductivity
US6193911B1 (en) * 1998-04-29 2001-02-27 Morton International Incorporated Precursor solution compositions for electronic devices using CCVD
DE102004001655A1 (en) 2004-01-12 2005-08-04 Interpane Entwicklungs- Und Beratungsgesellschaft Mbh & Co.Kg Substrate coated with a thermal barrier coating
DE102005061248B4 (en) * 2005-12-20 2007-09-20 Infineon Technologies Ag System carrier with surfaces to be embedded in plastic compound, method for producing a system carrier and use of a layer as a primer layer
DE102006029617A1 (en) 2006-06-23 2007-12-27 Verein zur Förderung von Innovationen durch Forschung, Entwicklung und Technologietransfer e.V. (Verein INNOVENT e.V.) Process for modifying the surface properties of glass

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4401474A (en) * 1979-12-03 1983-08-30 Ppg Industries, Inc. Pyrolytic coating reactant for defect and durability control
US4292347A (en) * 1979-12-03 1981-09-29 Ppg Industries, Inc. Pyrolytic coating reactant for defect and durability control
US6207522B1 (en) * 1998-11-23 2001-03-27 Microcoating Technologies Formation of thin film capacitors
DE102006045617B4 (en) * 2006-09-22 2010-06-10 Innovent E.V. Technologieentwicklung Process for producing an inorganic-inorganic gradient composite layer
DE102007011865A1 (en) * 2007-03-08 2008-09-18 Verein zur Förderung von Innovationen durch Forschung, Entwicklung und Technologietransfer e.V. (Verein INNOVENT e.V.) Production of electrochromic or gasochromic tungsten oxide layers on substrates comprises adding precursor to mixture of combustible gas and oxidizer and feeding product to burner, oxidized product being deposited on substrate
GB2451130B (en) * 2007-07-20 2011-08-03 Saint Gobain Deposition of metals by combustion CVD coating at atmospheric pressure

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4320931A1 (en) 1992-10-21 1994-04-28 Solvay Deutschland Deposition of layers with high specific electrical conductivity
US6193911B1 (en) * 1998-04-29 2001-02-27 Morton International Incorporated Precursor solution compositions for electronic devices using CCVD
DE102004001655A1 (en) 2004-01-12 2005-08-04 Interpane Entwicklungs- Und Beratungsgesellschaft Mbh & Co.Kg Substrate coated with a thermal barrier coating
DE102005061248B4 (en) * 2005-12-20 2007-09-20 Infineon Technologies Ag System carrier with surfaces to be embedded in plastic compound, method for producing a system carrier and use of a layer as a primer layer
DE102006029617A1 (en) 2006-06-23 2007-12-27 Verein zur Förderung von Innovationen durch Forschung, Entwicklung und Technologietransfer e.V. (Verein INNOVENT e.V.) Process for modifying the surface properties of glass

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
H. J. Gläser, Dünnfilmtechnologie auf Flachglas, Schorndorf, Verlag Karl Hofman, 1999

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011076203A1 (en) 2009-12-22 2011-06-30 Rent A Scientist Gmbh Formulation comprising metal nanoparticles
DE102009059276A1 (en) 2009-12-22 2011-06-30 Rent-a-Scientist GmbH, 93059 Formulation with metal nanoparticles
DE102010030301A1 (en) 2010-06-21 2011-12-22 Solayer Gmbh Substrate with superficially structured surface electrode
DE102010024521A1 (en) * 2010-06-21 2011-12-22 Innovent E.V. Method for increasing the translucency of a substrate
WO2011161038A1 (en) 2010-06-21 2011-12-29 Innovent E.V. Method for increasing the translucency of a substrate
WO2011161010A2 (en) 2010-06-21 2011-12-29 Solayer Gmbh Substrate with superficially structured surface electrode for a solar cell and method for producing said substrate
DE102012003943A1 (en) 2012-02-24 2013-08-29 Innovent E.V. Technologieentwicklung Preparing antimicrobial nano-layers on substrate material, in the form of e.g. fiber- or yarn materials, comprises surface modifying the substrate material by flame-pyrolysis process, and depositing a thin layer on the substrate material

Also Published As

Publication number Publication date
DE102008025108B4 (en) 2012-02-23
WO2009140961A1 (en) 2009-11-26
EP2283168A1 (en) 2011-02-16

Similar Documents

Publication Publication Date Title
DE102006014796B4 (en) Highly resilient low-E coating system for transparent substrates
EP1514851B1 (en) Protective coating for a body as well as process and plant unit for preparing protective coatings
EP3134756B1 (en) Temperature- and corrosion-stable surface reflector
DE102010004741B4 (en) Process for manufacturing a composite material and kitchen utensil
DE69222079T2 (en) Applying pyrolyzed layers with improved performance and glass pane provided with such a layer
EP2261185A2 (en) Solar glass panel with barrier coating and method for producing same
DE102009016708B4 (en) Solar absorber coating system and method for its production
EP1765921B1 (en) Multilayer structure for polymers
DE3329504A1 (en) HEAT WAVE SHIELDING LAMINATION
DE102008060074A1 (en) Transparent conductive film
DE102011116191A1 (en) Multi-layer systems for selective reflection of electromagnetic radiation from the wavelength spectrum of sunlight and method for its production
EP2668695A1 (en) Radar-transparent coating
DE69023369T2 (en) High temperature resistant spray coating on glass.
DE102008025108A1 (en) Process for the production of nanoscale electrically conductive multilayer systems
DE102007025151A1 (en) Coating method comprises producing plasma jet from process gas and introducing precursor material into it, coating being deposited from jet on to substrate or existing coating on it and substrate being heated
EP4347254A1 (en) Glazing unit having a metal-based coating and a protective layer at the margin
DE68903980T2 (en) ELECTRO-CONDUCTIVE GLASS AND METHOD FOR THE PRODUCTION THEREOF.
EP2714607B1 (en) Method and device for coating a float glass strip
DE102008009337B4 (en) Process for producing a transparent conductive layer
DE102007039645A1 (en) Coating or modifying surface of organic or inorganic wires, fibers or assemblies of them comprises exposing them to flame, plasma or stream of hot gas containing layer-forming organic or inorganic components
EP2933354A2 (en) Household device construction device
DE102007011865A1 (en) Production of electrochromic or gasochromic tungsten oxide layers on substrates comprises adding precursor to mixture of combustible gas and oxidizer and feeding product to burner, oxidized product being deposited on substrate
DE112021004623T5 (en) GLASS OBJECT
DE102013104212A1 (en) Bird protection glass used for exterior glazing, has bird-resistant coating comprising nitride(s) of titanium, zinc, tin, strontium-titanium, tungsten-bismuth, iron, silver, iron-silver, niobium, zirconium, tantalum or their alloy
DE102012215059B4 (en) Protective layer for an IR-reflecting layer system, IR-reflecting layer system and method for the production thereof

Legal Events

Date Code Title Description
OP8 Request for examination as to paragraph 44 patent law
R016 Response to examination communication
R018 Grant decision by examination section/examining division
R020 Patent grant now final

Effective date: 20120524

R119 Application deemed withdrawn, or ip right lapsed, due to non-payment of renewal fee
R119 Application deemed withdrawn, or ip right lapsed, due to non-payment of renewal fee

Effective date: 20141202