DE10131932C2 - Process for producing a heat-reflecting layer system for transparent substrates and layer system produced thereafter - Google Patents

Process for producing a heat-reflecting layer system for transparent substrates and layer system produced thereafter

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Publication number
DE10131932C2
DE10131932C2 DE10131932A DE10131932A DE10131932C2 DE 10131932 C2 DE10131932 C2 DE 10131932C2 DE 10131932 A DE10131932 A DE 10131932A DE 10131932 A DE10131932 A DE 10131932A DE 10131932 C2 DE10131932 C2 DE 10131932C2
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Prior art keywords
layer
proportion
reflective
metal
silver
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DE10131932A
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German (de)
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DE10131932A1 (en
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Volker Kirchhoff
Torsten Kopte
Ullrich Hartung
Matthias Fahland
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Priority claimed from DE10046810A external-priority patent/DE10046810C5/en
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Priority to DE10131932A priority Critical patent/DE10131932C2/en
Priority to EP02013422A priority patent/EP1273558A1/en
Publication of DE10131932A1 publication Critical patent/DE10131932A1/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3626—Surface 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 one layer at least containing a nitride, oxynitride, boronitride or carbonitride
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3644—Surface 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3652—Surface 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 coating stack containing at least one sacrificial layer to protect the metal from oxidation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3657—Surface 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
    • C03C17/366—Low-emissivity or solar control coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3681—Surface 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface 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
    • C03C17/3602—Surface 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
    • C03C17/3694—Surface 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 one layer having a composition gradient through its thickness
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C03C2217/91—Coatings containing at least one layer having a composition gradient through its thickness

Description

Die Erfindung betrifft ein Verfahren zur Herstellung eines wärmereflektierenden Schicht­ systems für transparente Substrate, vorzugsweise Glas, welches aus mindestens einer elektrisch hoch leitfähigen Funktionsschicht, an welche sich mindestens eine metallische Blockerschicht - auch Zwischenschicht genannt - unmittelbar anschließt, und mehreren hochbrechenden Entspiegelungsschichten besteht, nach Patent 100 46 810. Das Schichtsystem wird auch als low-e-Schichtsystem bezeichnet.The invention relates to a method for producing a heat-reflecting layer systems for transparent substrates, preferably glass, which consists of at least one electrically highly conductive functional layer to which at least one metallic Blocker layer - also called intermediate layer - immediately adjoins, and several highly refractive antireflection coatings, according to patent 100 46 810. The layer system is also referred to as a low-e layer system.

Derartige Schichtsysteme auf Glas eignen sich für einen anschließenden Härt- bzw. Biege­ prozess der beschichteten Glasscheibe, z. B. für Fahrzeuge, vorzugsweise auch als wärme­ dämmende Sicherheitsverglasung.Layer systems of this type on glass are suitable for subsequent hardening or bending process of the coated glass pane, e.g. B. for vehicles, preferably also as heat insulating safety glazing.

Es sind eine Vielzahl solcher wärmereflektierenden Schichtsysteme bekannt. Das Schicht­ system besteht allgemein aus Funktionsschicht, Grund- und Deckschicht, wobei letztere als Entspiegelungsschichten dienen. Die einzelnen Schichten können sich im Gesamtsystem mehrfach wiederholen. Als Funktionsschicht für die Wärmereflexion werden üblicherweise Edelmetalle - vorzugsweise Silber - aufgrund ihres guten selektiven Reflexionsvermögens schon bei geringen Schichtdicken verwendet. Die Entspiegelungsschichten dienen zur Verbesserung der optischen Eigenschaften im sichtbaren Längenwellenbereich und sind mindestens auf einer Seite der Funktionsschicht oder auf der über der Funktionsschicht aufgebrachten Blockerschicht angeordnet. Die Entspiegelungsschicht beeinflusst entscheidend das Gesamtschichtsystem hinsichtlich dessen elektrischer Eigenschaft, d. h. Leitfähigkeit, der mechanischen Eigenschaften, z. B. Kratzfestigkeit und chemischer Eigenschaften, z. B. Beständigkeit gegen Säuren.A large number of such heat-reflecting layer systems are known. The layer system generally consists of a functional layer, base and top layer, the latter as Anti-reflective layers serve. The individual layers can be in the overall system Repeat several times. Usually used as a functional layer for heat reflection Precious metals - preferably silver - due to their good selective reflectivity already used for thin layers. The anti-reflective layers are used for Improvement of the optical properties in the visible wavelength range and are at least on one side of the functional layer or on the one above the functional layer applied blocker layer arranged. The anti-reflective layer affects decisive is the overall layer system with regard to its electrical property, d. H. Conductivity, mechanical properties, e.g. B. scratch resistance and chemical Properties, e.g. B. Resistance to acids.

Es ist bekannt, zur Verbesserung der optischen Eigenschaften, insbesondere zur Erhöhung der Transmission im sichtbaren Bereich, hochbrechende Entspiegelungsschichten, vorzugsweise dielektrische Metalloxide oder -nitride, oberhalb und/oder unterhalb der Funktionsschicht anzuordnen. Beim Aufbringen eines Metalloxids als Entspiegelungsschicht auf die Funktionsschicht und beim Biegen und/oder Härten beschichteter Glasscheiben mit dem damit verbundenen Erwärmem kommt es zur Oxidation der Funktionsschicht, zur Diffusion des Silbers in die Entspiegelungsschicht, zur Diffusion von Komponenten der Entspiegelungsschicht in das Silber und/oder zu Agglomerationen innerhalb der Funktionsschicht. Durch diese Effekte werden das Reflexionsvermögen der Beschichtung für Wärmestrahlung sowie die Transmission im sichtbaren Bereich verringert.It is known to improve the optical properties, in particular to increase it the transmission in the visible range, highly refractive anti-reflective layers, preferably dielectric metal oxides or nitrides, above and / or below the Arrange functional layer. When applying a metal oxide as an anti-reflective coating on the functional layer and when bending and / or hardening coated glass panes the associated heating leads to the oxidation of the functional layer, to Diffusion of the silver into the anti-reflective coating, for the diffusion of components of the Anti-reflective coating in the silver and / or to agglomerations within the  Functional layer. Through these effects, the reflectivity of the coating for Thermal radiation and the transmission in the visible range reduced.

Zur Vermeidung dieser Nachteile ist es bekannt, die Funktionsschicht durch geeignete Materialien - Blocker genannt - vor der teilweisen Zerstörung zu schützen, indem eine Blockerschicht oberhalb und/oder unterhalb der Funktionsschicht angeordnet wird (DE 38 25 671 A1; US 4,894,290; DE 196 32 788 A1).To avoid these disadvantages, it is known to use suitable functional layers Protect materials - called blockers - from partial destruction by one Blocker layer is arranged above and / or below the functional layer (DE 38 25 671 A1; US 4,894,290; DE 196 32 788 A1).

Als weitere Möglichkeit, die teilweise Oxidation der Funktionsschicht zu unterdrücken, ist der Einsatz von Nitriden als Entspiegelungsschicht bekannt (US 5,837,108). Jedoch kann auch hier, insbesondere bei härt- oder biegbaren Schichtsystemen, im Allgemeinen nicht gänzlich auf die Anordnung einer Blockerschicht verzichtet werden. Außerdem ist die Brechzahl von Metallnitriden im Allgemeinen deutlich geringer als die von Metalloxiden, was zu einer geringeren Entspiegelung (Bandbreite) führt.Another possibility is to suppress the partial oxidation of the functional layer the use of nitrides as an anti-reflective coating is known (US 5,837,108). However, can generally also not here, particularly in the case of hardenable or bendable layer systems the arrangement of a blocker layer can be dispensed with entirely. Besides, that is Refractive index of metal nitrides is generally significantly lower than that of metal oxides leads to less anti-reflective coating (bandwidth).

Es ist bekannt, zur Verbesserung der Eigenschaften der Entspiegelungsschicht diese nicht nur als eine einzige Schicht anzuordnen, sondern ein Teilschichtsystem aus mindestens zwei Schichten zu verwenden, die meist aus dielektrischem Material sind (DE 39 41 026 A1; DE 39 41 027 A1). Es wurde jedoch festgestellt, dass durch die Kombination der zwei einzeln bewerteten Eigenschaften der Einzelschichten als ein Teilschichtsystem insbesondere die mechanische Beständigkeit negativ beeinträchtigt wird.It is known not to improve the properties of the anti-reflective coating to be arranged only as a single layer, but a sub-layer system consisting of at least two To use layers, which are mostly made of dielectric material (DE 39 41 026 A1; DE 39 41 027 A1). However, it was found that by combining the two individually assessed properties of the individual layers as a partial layer system in particular the mechanical resistance is adversely affected.

Es wurde zur Beseitigung der Mängel des Standes der Technik bereits mit dem Patent 100 46 810 ein wärmereflektierendes Schichtsystem für transparente Substrate vorgeschlagen, welches aus mindestens einer Entspiegelungsschicht, mindestens einer Funktionsschicht aus Silber und mindestens einer auf einer Seite der Funktionsschicht aufgebrachten Blockerschicht aus einem Metall oder einer Metalllegierung und mindestens einer Deckschicht besteht, die durch Aufdampfen oder Sputtern im Vakuum derart aufgebracht werden, indem das Aufbringen der Metallteilchen für die Blockerschicht während der Beschichtung so geregelt wird, dass aus dem Silber der Funktionsschicht und dem Metall der Blockerschicht eine Gradientenschicht als Blockerschicht entsteht, dass bei der Herstellung einer Entspiegelungsschicht aus mehreren Metalloxid-Einzelschichten die Zuführung der aufzubringenden Metalloxidteilchen für die Einzelschichten so geregelt wird, dass eine Gradientenschicht entsteht und dass bei der Herstellung der Gradientenschichten die Regelung derart erfolgt, dass sich der Anteil des Schichtmaterials der in der Beschichtungsfolge zuerst aufzubringenden Schicht von 100% auf 0% und gegenläufig der Anteil des Schichtmaterials der darauf folgenden Schicht von 0% auf 100% ändert. Das nach dem vorgeschlagenen Verfahren hergestellte Schichtsystem besteht aus einer Blockerschicht aus einem Metall oder einer Metalllegierung, die mit dem Silber der Funktionsschicht eine Gradientenschicht bildet, und wenn die Entspiegelungsschicht aus mehreren Einzelschichten besteht, ist sie eine Gradientenschicht aus den Metalloxiden der Einzelschichten.It has been used to remedy the shortcomings of the prior art with the patent 100 46 810 a heat reflective layer system for proposed transparent substrates, which consists of at least one anti-reflective layer, at least a functional layer made of silver and at least one on one side of the functional layer applied blocker layer made of a metal or a metal alloy and at least a cover layer, which is formed by vapor deposition or sputtering in a vacuum can be applied by applying the metal particles for the blocker layer during the coating is regulated so that the silver of the functional layer and a gradient layer is formed as a blocker layer in the metal of the blocker layer, that at the production of an anti-reflective coating from several individual metal oxide layers Supply of the metal oxide particles to be applied for the individual layers is regulated in such a way that a gradient layer is created and that in the production of the gradient layers the regulation takes place in such a way that the proportion of the layer material in the  Coating sequence first layer to be applied from 100% to 0% and in opposite directions the proportion of the layer material of the subsequent layer changes from 0% to 100%. The layer system produced by the proposed method consists of a Blocker layer made of a metal or a metal alloy, which with the silver of the Functional layer forms a gradient layer, and when the anti-reflective layer is off consists of several individual layers, it is a gradient layer made of the metal oxides Individual layers.

Die Verwendung von Metalloxiden für die Entspiegelungsschicht bzw. -schichten stellt keine optimale Lösung dar.The use of metal oxides for the anti-reflective layer or layers is not a problem optimal solution.

Der Erfindung liegt die Aufgabe zugrunde, das Verfahren zur Herstellung eines wärme­ reflektierenden Schichtsystems nach dem Patent 100 46 810 bezüglich des verwendeten Materials weiter auszugestalten. Es soll auch farbneutral, mechanisch hoch belastbar, chemisch beständig, langzeitstabil und temperaturbeständig sein. Das Schicht­ system soll ohne Verringerung der Lichttransmission bzw. des Emissionsvermögens härt- und biegbar sein.The invention has for its object the method for producing a heat reflective layer system according to the patent 100 46 810 with respect to further used material. It should also be color neutral, mechanically high resilient, chemically stable, long-term stable and temperature-resistant. The layer system should harden without reducing light transmission or emissivity and be flexible.

Erfindungsgemäß wird die Aufgabe nach Anspruch 1 und 2 gelöst.According to the invention the object is achieved according to claims 1 and 2.

Das Wesen der Erfindung besteht darin, dass beim Aufbau der Entspiegelungsschicht aus mehreren Einzelschichten gemäß dem Patent 100 46 810 diese aus unter­ schiedlichen Metallnitriden bestehen und der Materialanteil einer Schicht von anfangs 100% bis 0% reduziert und der Anteil an Material der folgenden Schicht wird umgekehrt von 0% bis zu 100% erhöht. Es wurde festgestellt, dass eine derartige Gradientenschicht aus Metallnitriden die Gesamteigenschaften des Systems ebenfalls verbessert.The essence of the invention is that when building up the anti-reflective coating several individual layers according to the patent 100 46 810 these from below Different metal nitrides exist and the material content of a layer from the beginning 100% to 0% reduced and the proportion of material in the following layer is reversed increased from 0% to 100%. It was found that such a gradient layer made of metal nitrides also improves the overall properties of the system.

Das erfindungsgemäße Verfahren wird bekannterweise derart ausgeführt, dass die Beschichtungsstationen zur Herstellung der Entspiegelungsschicht für jede Metall­ nitridschicht in der Beschichtungsanlage räumlich so angeordnet werden, dass sich die Verteilungen der aufzubringenden Teilchen auf der Substratebene bzw. der vorangegangen bereits aufgebrachten Schicht teilweise überlagern. Die Eigenschaften der Gradientenschicht lassen sich einfach mit Mitteln der Prozessführung, z. B. Abstand der Beschichtungs­ stationen, Parameter der Energieeinspeisung, Verhältnis der eingespeisten Leistungen, beeinflussen.The method according to the invention is known to be carried out in such a way that the Coating stations for the production of the anti-reflective coating for every metal nitride layer in the coating system so that the Distributions of the particles to be applied on the substrate level or the previous one Partially overlay already applied layer. The properties of the gradient layer can be easily with means of process control, e.g. B. Distance of the coating stations, parameters of energy feed-in, ratio of the feed-in powers, influence.

An einem Ausführungsbeispiel wird die Erfindung beschrieben. Die zugehörige Zeichnung zeigt ein Schichtsystem mit als Gradientenschicht ausgebildeter Funktions- und Blocker­ schicht und einseitig angeordneter Entspiegelungsschicht.The invention is described using an exemplary embodiment. The associated drawing shows a layer system with function and blockers designed as a gradient layer layer and one-sided anti-reflective layer.

Das erfindungsgemäße Verfahren wird wie folgt ausgeführt:
Die Figur zeigt ein Schichtsystem, bei welchem auf der Glasscheibe in einem ersten Verfahrensschritt eine Entspiegelungsschicht 1 als Gradientenschicht aus quasi zwei Einzelschichten aus AlN Und Si3N4 aufgebracht ist. Der Anteil des zuerst aufgebrachten Materials - AlN - geht während des Aufbringens von einem Anteil von 100% kontinuierlich über die Dicke der Schicht auf 0% zurück, während der Anteil des nächstfolgenden Materials - Si3N4 - gegenläufig von 0% auf 100% ansteigt. Danach wird die Funktions­ schicht 2 aus Ag aufgebracht und auf der Funktionsschicht 2 aus Ag die Blockerschicht 3 als eine durchgehende Gradientenschicht aus NiCr und Ag. Innerhalb dieser Blockerschicht 3 beträgt der Gradient beider Materialien 0% bis 100% und umgekehrt. Der Übergang von der Funktionsschicht 2 zur Blockerschicht 3 ist nicht fließend, sondern es liegt eine, wenn auch nicht exakt feststellbare Trennung beider Schichten vor. Darauf wird eine obere Entspiegelungsschicht 4 aus TiO2 aufgebracht.The method according to the invention is carried out as follows:
The figure shows a layer system in which, in a first method step, an anti-reflective layer 1 is applied to the glass pane as a gradient layer composed of quasi two individual layers made of AlN and Si 3 N 4 . The proportion of the first applied material - AlN - continuously decreases during the application from a proportion of 100% over the thickness of the layer to 0%, while the proportion of the next material - Si 3 N 4 - increases in the opposite direction from 0% to 100% , Thereafter, the function is applied from 2 Ag and on the functional layer 2 from the Ag blocker layer 3 as a continuous gradient layer of NiCr and Ag. Layer Within this blocker layer 3 , the gradient of both materials is 0% to 100% and vice versa. The transition from functional layer 2 to blocker layer 3 is not smooth, but there is a separation of the two layers, although it cannot be determined exactly. An upper anti-reflective layer 4 made of TiO 2 is applied thereon.

Claims (2)

1. Verfahren zur Herstellung eines wärmereflektierenden Schichtsystems für transparente Substrate, insbesondere Glas, bestehend aus mindestens einer Entspiegelungsschicht, die aus mehreren Einzelschichten besteht, mindestens einer Funktionsschicht aus Silber und mindestens auf einer Seite dieser Funktionsschicht aufgebrachten metalli­ schen Blockerschicht, die aus dem Silber und dem Metall als Gradientenschicht aus­ geführt ist und wobei sich der Anteil des metallischen Schichtmaterials der ersten Schicht von 100% auf 0% und gegenläufig der Anteil des folgenden metallischen Schichtmaterials von 0% auf 100% ändert, sowie mindestens einer Entspiegelungs- oder Deckschicht, wobei die Schichten durch Aufdampfen oder Sputtern im Vakuum aufgebracht werden, nach Patent 100 46 810, dadurch gekennzeichnet, dass die Einzelschichten der Entspiegelungsschicht aus unterschiedlichen Metallnitriden hergestellt werden und die Zuführung der aufzubringenden Metallnitridteilchen für die Einzelschichten so geregelt wird, dass eine Gradientenschicht gebildet wird, deren Anteil des einen Metallnitrids einer Schicht von 100% auf 0% und dazu gegenläufig das Metallnitrid der anderen Schicht von 0% auf 100% verändert werden.1. A method for producing a heat-reflecting layer system for transparent substrates, in particular glass, consisting of at least one anti-reflective layer, which consists of several individual layers, at least one functional layer made of silver and at least one side of this functional layer applied metallic blocker layer consisting of the silver and the Metal is performed as a gradient layer and the proportion of the metallic layer material of the first layer changes from 100% to 0% and, in the opposite direction, the proportion of the following metallic layer material changes from 0% to 100%, as well as at least one anti-reflective or top layer, the layers be applied by vapor deposition or sputtering in a vacuum, according to patent 100 46 810, characterized in that the individual layers of the anti-reflective layer are produced from different metal nitrides and the supply of the metal nitride particles to be applied for the single layer is regulated in such a way that a gradient layer is formed, the proportion of one metal nitride of one layer of which is changed from 100% to 0% and, in the opposite direction, the metal nitride of the other layer is changed from 0% to 100%. 2. Wärmereflektierendes Schichtsystem, hergestellt nach Anspruch 1, bestehend aus mindestens einer Entspiegelungsschicht aus mehreren Einzelschichten, mindestens einer Funktionsschicht aus Silber, mindestens einer auf einer Seite der Funktions­ schicht aufgebrachten metallischen Blockerschicht als Gradientenschicht aus diesem Metall und Silber, wobei sich der Anteil des Metalls der Blockerschicht zum Silber über seine Dicke von 100% auf 0% und gegenläufig der Anteil des Silbers zum Metall der Blockerschicht von 0% auf 100% kontinuierlich oder diskontinuierlich ändert, sowie mindestens einer Entspiegelungs-, Haft-, Schutz- und/oder Deckschicht, nach Patent 100 46 810, dadurch gekennzeichnet, dass die Einzelschichten der Entspiegelungsschicht aus einem Metallnitrid bestehen und eine Gradientenschicht sind, deren Anteil des Schichtmaterials der in der Beschichtungsfolge zuerst auf­ zubringenden Schicht von 100% auf 0% und gegenläufig der Anteil des Schicht­ materials der darauf folgenden Schicht von 0% auf 100% kontinuierlich oder dis­ kontinuierlich ändert.2. Heat reflecting layer system, produced according to claim 1, consisting of at least one anti-reflective coating from several individual layers, at least a functional layer made of silver, at least one on one side of the functional layer applied metallic blocker layer as a gradient layer from this Metal and silver, the proportion of the metal in the blocker layer becoming silver its thickness from 100% to 0% and the opposite proportion of silver to metal Blocker layer changes continuously or discontinuously from 0% to 100%, as well at least one anti-reflective, adhesive, protective and / or top layer, according to patent 100 46 810, characterized in that the individual layers of the Anti-reflective layer consist of a metal nitride and a gradient layer are, the proportion of the layer material that in the coating sequence first layer to be added from 100% to 0% and the opposite proportion of the layer materials of the subsequent layer from 0% to 100% continuously or dis changes continuously.
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US10696584B1 (en) * 2019-11-26 2020-06-30 Guardian Europe S.A.R.L. Coated article with low-E coating having protective contact layer including Ag, Ni, and Cr for protecting silver based IR reflecting layer(s), and method of making same

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