DE102012207556A1 - IR-reflecting, transparent layer system and method for its production - Google Patents

IR-reflecting, transparent layer system and method for its production

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Publication number
DE102012207556A1
DE102012207556A1 DE201210207556 DE102012207556A DE102012207556A1 DE 102012207556 A1 DE102012207556 A1 DE 102012207556A1 DE 201210207556 DE201210207556 DE 201210207556 DE 102012207556 A DE102012207556 A DE 102012207556A DE 102012207556 A1 DE102012207556 A1 DE 102012207556A1
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Prior art keywords
layer
functional layer
arrangement
reflecting
infrared radiation
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DE201210207556
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German (de)
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Dr. Köckert Christoph
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Von Ardenne Anlagentechnik GmbH
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Von Ardenne Anlagentechnik GmbH
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Priority to DE201210207556 priority Critical patent/DE102012207556A1/en
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Application status is Withdrawn legal-status Critical

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    • 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
    • C03C17/3613Coatings of type glass/inorganic compound/metal/inorganic compound/metal/other
    • 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
    • C03C17/3626Surface 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
    • 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
    • C03C17/3639Multilayers containing at least two functional metal layers
    • 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
    • C03C17/3652Surface 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
    • 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
    • C03C17/3681Surface 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

Abstract

The invention relates to an infrared radiation-reflecting transparent layer system on a transparent, dielectric substrate S0 and to a method for producing the same, which viewed from the substrate S0 has a base layer arrangement GA with a dielectric base layer GAG, an overlying functional layer arrangement UFA with a metallic functional layer UFAF and a blocking layer UFAB and a cover layer arrangement DA comprises. In order to reduce the material costs of the layer system without loss in the optical, mechanical and thermal properties, at least one functional layer contains UFAF, MFAF, OFAF copper and at least one functional layer UFAF, MFAF, OFAF silver.

Description

  • The invention generally relates to a heat-treatable infrared radiation (IR) -reflecting, transparent layer system which contains at least two metallic IR reflection layers on a transparent, dielectric substrate, and to a method for producing such a layer system.
  • Functionally, an IR-reflecting layer system, hereinafter also referred to as layer system, characterized by its low emissivity and associated high reflectivity and low transmission in the spectral IR range (wavelengths of >> 3μm). At the same time a high (low-E layer systems) or targeted reduced transmission (low-E-Sun layer systems) in the visible light range should be achieved. It thus has a steep drop in transmission and a large increase in reflection in the transition from visible light to near infrared. Due to their emission behavior, such layer systems are generally referred to as low-E layer systems.
  • The low-E-Sun coating systems are used for architectural glazing, as solar control glazing, where an energy input through the glazing predominates and a low energy transmission and thus a high selectivity of the glazing used is advantageous. In contrast, the low-E layer systems described above are used for glazing in climatic regions with predominant energy loss through the glazing. In addition to the structure and the materials of the various IR-reflecting layer systems and their location in architectural glazing is different. In the following, both types of IR-reflecting layer systems will be referred to simply as a layer system and, unless otherwise described, should comprise low-E and low-E-Sun layer systems.
  • A layer system has transparent and partially absorbing, functionally distinguishable layer arrangements in order to achieve the described properties.
  • The term "layer arrangement" as described generally comprises more than one layer, but also includes that a layer arrangement consists only of a single layer, which realizes the respective function. The assignment of individual layers to the layer arrangements is not always unambiguous, since each layer has an influence on the adjacent layers as well as on the entire system. Generally, a layer is assigned based on its function.
  • In general, a layer system, viewed from the substrate upwards, initially comprises a base layer arrangement which primarily serves as an intermediary between the substrate and the further layer sequence, in particular the adhesion of the system to the glass. The layers of the basecoat assembly may also affect the properties of the layer system as a whole, such as e.g. the chemical and / or mechanical resistance and / or the adjustment of optical properties.
  • The base layer arrangement is followed by a functional layer arrangement which comprises the IR reflection layer and optionally further layers which support this function and enable the influence of their optical, chemical, mechanical and electrical properties or serve for adhesion. Such supplemental layers are e.g. such as blocker, seed or interface layers, which serve to deposit and / or adjust electrical and optical properties of adjacent layers. With a suitable choice of material, several of the functions can be realized by a layer. Thus, the arrangement of a lower blocker layer may result in an underlying seed layer being eliminated.
  • The high reflection in the IR range is achieved for the said layer systems generally by one or more metallic IR reflective layers. As a rule, the edge described in the spectral transmission and reflection behavior becomes steeper as the number of IR reflection layers increases, i. the selectivity increases, which is why layer systems with two or more IR reflective layers are increasingly being used.
  • Pure silver or silver alloys are typically used for the IR reflective layer to make low-emissivity layer systems for architectural glass applications. This material has high reflectivity even at low layer thicknesses, especially in the infrared range, combined with low absorption in the visible spectral range of the light. The disadvantage is the very high and steadily rising price for silver. A simple low-E layer system usually contains an approximately 10-15nm thick silver layer. In multiple low-E layer systems with improved thermal properties, e.g. lower emissivity, a lower g-value or increased selectivity, the total silver thickness is approximately in line with the number of silver layers and thus also the material costs. The silver costs make up the bulk of the material costs in the production of such layer systems.
  • Frequently, in the course of the production of the layer system, different temperature loads occur in already applied layer sequences, which are due to an energy input associated with the deposition or different treatment steps of deposited layers. In addition, IR-reflecting layer systems for curing and / or deformation of the substrate are also subjected to annealing processes. In this case, they have such a layer sequence with such layer properties, which make it possible to heat-treat a substrate carrying the layer system and to keep occurring changes in the optical, mechanical and chemical properties of the layer system within defined limits. Depending on the application of a coated substrate, its layer system is exposed to different climatic conditions in the annealing process in different time regimes.
  • As a result of such thermal stresses, various processes which change the reflectivity of the IR reflection layer and the transmission of the layer system occur, in particular for the diffusion of components of the substrate or the antireflection coating into the IR reflection layer and vice versa, and consequently to oxidation processes in the IR reflection layer.
  • To avoid such diffusion and oxidation processes, a blocker layer is inserted on one or both sides of the IR reflection layer, which serves as a buffer for the diffusing components. These blocking layers are structured and arranged in accordance with the temperature load that occurs and protect the sensitive, often very thin IR reflection layer or the IR reflection layers from the influence of adjacent layers. By inserting one or more blocking layers, it is possible in particular to prevent the oxidation of the IR reflection layer of the layer system and the associated increase in surface resistance or even pronounced color shifts of the layer system during the coating processes themselves or as a result of the tempering process. For example, nickel and / or chromium-containing layers which include the IR-reflecting silver layers are known as blocking layers of temperature-capable layer systems. DE 035 43 178 A1 and EP 1 174 379 A1 ) or at least protect it on one side.
  • At the same time, the blocker layers are also useful to adjust the transmission of the layer system by having one or more blocker layers regularly underlying the IR reflective layer act as absorber layers. For this reason, low-E-Sun layer systems have at least one blocking layer. This is usually below the lowest, i. Substrate next IR reflection layer arranged.
  • In addition, it was found that the reflection and transmission properties of the layer system are also influenced by diffusion processes that emanate from the glass. In order to influence this, in particular for temperature-capable layer systems below the functional layer arrangement, regularly in the base layer arrangement, a barrier layer is introduced which prevents the diffusion of constituents of the glass, such as e.g. To reduce alkali metal ions in the layer system. Also, with such a barrier layer, quality problems that are due to undefined initial conditions in the raw glass, ie. H. fluctuating chemical composition of the glass, or other glass influences are due.
  • Layers of the cover layer arrangement close off the layer system and, like the base layer arrangement, can functionally affect the entire system. A cover layer arrangement comprises at least one mechanically and / or chemically stabilizing protective layer. This can itself or through complementary layers also influence the optical performance of the layer system, e.g. an antireflection coating using interference effects, so that optionally in conjunction with an antireflective base layer, the transmission can be increased. The cover layer arrangement usually consists of one or more layers of a dielectric oxide, nitride or oxynitride of a metal or of a semiconductor mostly having a high refractive index.
  • These dielectric materials are considered as non-absorbent materials, which qualifies them for the described optical function. In the case of transparent layer systems, high-refractive index materials are generally transparent materials whose refractive index is in the range from 1.8 to 2.7, in most cases even in the range of 1.9, preferably from 2.0 to 2.6. For comparison, the substrate, usually float glass, which has a low refractive index of about 1.52 on the other hand. As a result, materials below this range are low-refractive indexes up to values in the region of the substrate.
  • Such a so-called single-low E or single low E sun, which comprises only one functional layer arrangement, can be supplemented by insertion of one or more further functional layer arrangements (double, triple, or multi-low E or Low-E-Sun), which are arranged by coupling or interlayer arrangements over the first functional layer arrangement. The interlayer arrangements serve in particular anti-reflection in the visible range by functional separation of the two functional layer arrangements from one another and their mechanical connection with one another. In addition, with suitable Material combination is achieved by an interlayer arrangement and a mechanical stabilization of the layer system.
  • Another requirement for the architectural glazing is the color impression and its stability. Often, neutral or gray to blue substrate side reflection colors are desired, which should be independent of the viewing angle. Neutral colors in the CIE L * a * b * color system are characterized by a * and b * color values of approximately zero, while blue colors are characterized by negative b * color values and red colors by positive a * color values. Furthermore, in some applications, neutral or gray transmission colors may be required.
  • The object of the invention is to provide an IR-reflective layer system and a method for its production, which can be produced with lower material costs and thereby has comparable or better optical, mechanical and thermal properties compared to the silver-based layer systems.
  • To solve an IR-reflective layer system according to claim 1 and a method for its preparation according to claim 8 is given. In the dependent claims advantageous embodiments of the invention are described.
  • According to the invention, a copper-containing IR reflection layer is combined with a silver-containing IR reflection layer in an at least two IR reflection layers, which are also referred to below as functional layers. In the case of multiple low-E and multiple-low E-Sun layer systems, one or more of the silver layers can be replaced by copper layers. The silver layer can be partially or completely replaced by a copper layer, so that alternatively functional layers can be used, which consist of partial layers, one of which contains copper and another silver. Due to the partial use of copper instead of silver, comparable emissivities of the layer system and thus g or U values of the insulating glass unit can be achieved with the same layer thickness.
  • As a layer containing copper or silver, it should be understood here that such a material composition is that the essential constituent and the electro-optical characteristics are copper or silver or their alloys. This implies that technologically conditioned impurities or of technologically-caused admixtures leading to process control during deposition or, e.g. can be contained in the sputtering, are useful for the target production. Such impurities or technological admixtures are usually in the range of less than 1%, but may also be a few percent.
  • An advantage of the use of copper or copper-containing materials, in addition to the significantly lower material costs, is the dispersion properties of the refractive index and the extinction coefficient, which differ from those of silver, particularly in the visible range. The 1A and 1B respectively. 2A and 2 B show the wavelength-dependent transmission and reflection behavior of a 20nm thin copper or silver layer in the wavelength range of solar radiation from about 350nm to 2500nm.
  • It has been found that, despite the reddish color appearance of copper in coating systems with the desired low-E and low-E-Sun specifications in terms of transmission and emissivity, with suitable material and layer thickness combination of the individual layers of the layer system neutral transmission colors and also reflection lower overall reflection values can be achieved than would be possible with silver.
  • Another aspect of the invention is the higher absorption of copper in the visible region of the spectrum compared to silver, which reduces the light transmission of the layer system. Therefore, by the number and thickness of the copper layer or other transmission-increasing layers to set an optimum in the transmission. Alternatively, this effect can be specifically exploited for a low-E-Sun system. The low transmission in the low-E-Sun layer system, combined with low emissivity, can be easily achieved by using copper for at least one IR reflection layer. Emissivities in the range of less than 3% can already be achieved with double-low E systems. For low-E-Sun layer systems, by means of the number of functional layers containing copper and / or the thicknesses of at least one blocking layer, the transmission of the layer system to values in the range of 25 ≦ Y (T) ≦ 75% can also be achieved with a neutral color appearance. The reduction of the transmission by means of a blocking layer underneath an IR reflection layer can also be omitted, which results in both a waiver of this layer and in its use, e.g. for temperature-capable layer systems for realizing the protective function described above or for setting the transmission, further options for the optical and thermal behavior of the layer system result.
  • If, according to further embodiments of the layer system, a silver-containing functional layer is arranged above the functional layer containing copper, for the Transmission and color values of the substrate-side reflection and thus for the intensity of a substrate-side color appearance better or at least similar values are achieved compared to known layer systems. For example, in a multiple low-E or multiple low-E sun, each additional functional layer disposed over the copper-containing layer may be silver-containing or silver-plated. In particular, in this embodiment, neutral color appearance of the coated substrate have been achieved with required emissivity up to less than 2%.
  • In an arrangement of the silver-containing over the copper-containing functional layer, the layer system according to the invention has a neutral to blue substrate-side reflection color, i. the a * (Rg) and b * (Rg) color values of the CIE L * a * b * substrate side reflection color system are in the range of -5 ≤ a * ≤ 1 and -10 ≤ b * ≤ 1. This property can e.g. can be achieved via a layer thickness variation of the individual layers of the layer system as a pure color optimization or via a layer thickness variation of an interlayer arrangement. A layer thickness variation of an interlayer arrangement also allows the color optimization over almost the entire viewing angle, so that a color change in the reddish color space depending on the viewing angle does not occur.
  • The protection of the functional layers in the manner known for silver by a barrier layer underlying the lowest functional layer and by blocking layers arranged below and / or above the individual functional layers is also necessary for maintaining the IR-reflecting properties of the copper layer. Sufficient inhibition of the degradation of a copper-containing functional layer can be achieved by a dense, e.g. nitrogen-containing barrier layer against diffusion processes from the substrate in conjunction with a higher compared to silver layer thickness and / or arranged over the functional layer blocker layer and a chemically stable top layer arrangement can be achieved.
  • The materials which can be used functionally and structurally for a barrier layer depend essentially on these properties, specifically with regard to the diffusion processes to be expected, so that the appropriate materials can be determined by experiments for the given substrate-layer combinations and thermal requirements. With respect to sodium ion diffusion from glass, e.g. found that some metal oxides, e.g. Tin oxide, zinc stannate or titanium oxide show only a negligible barrier effect.
  • Depending on the material used, the base layer may well be highly refractive. In this case, the base layer can simultaneously serve the anti-reflection.
  • In addition, according to one embodiment of the invention, at least one functional layer arrangement (UFA, MFA, OFA) also containing the copper may comprise a blocking layer (UFAB) of a metal, a metal mixture or metal alloy or of a substoichiometric or stoichiometric oxide, nitride or oxynitride thereof, for protecting the functional layer (UFAF) against oxidation and diffusion processes.
  • If the barrier effect by the base layer already sufficient stabilization of the layer system against thermal influences, which are justified by the substrate, can be achieved, then it is not necessary according to an embodiment of the invention, for example, for a desired higher transmission of the layer systems to arrange a lower blocker layer , This possibility has a positive effect on the transmission in the visible spectral range, but without sacrificing thermal stability. Thus, of the blocking layers arranged on both sides of a functional layer, only the upper one remains, which lies above the functional layer and forms a protection against diffusion and associated oxidation processes of layers deposited over the functional layer.
  • Incidentally, the configuration of the layer system according to the invention is based on the known requirements, so that further layers can be arranged. These include interlayer arrangements. These regularly comprise one or more intermediate layers and may consist of various dielectric materials of oxides, nitrides or oxynitrides of metals, metal alloys or metal mixtures or semiconductors or compounds thereof.
  • Furthermore, a seed layer can be arranged below functional layers, also as the upper termination of an interlayer arrangement. A seed layer is suitable for positively influencing the deposition and the reflection properties of the IR-reflecting functional layer. With a seed layer, the adhesion of the IR-reflecting functional layer deposited over the seed layer can be improved and the sheet resistance reduced and thus the IR reflection properties can be improved. The seed layer consists of a metal or of an oxide or nitride of a metal or a metal mixture or metal alloy and is incorporated as a layer in the sense of a seed layer, which influences the layer structure of the functional layer during the deposition in such a way that the desired, low Sheet resistance is achieved. Is under the Functional layer arranged a blocking layer, the seed layer can also be omitted or it is arranged between the lower blocker layer and the functional layer.
  • The invention will be explained in more detail with reference to an embodiment. In the accompanying drawing shows in the
  • 1A . 1B Reflection and transmission of a copper layer in the solar radiation area,
  • 2A . 2 B Reflection and transmission of a silver layer in the solar radiation area,
  • 3 a layer sequence of a double-low E-Sun layer system,
  • 3 represents an inventive IR-reflective layer system with two functional layer arrangements FA (Double-Low-E), the individual layers described below are deposited on a substrate S0 successively in a vacuum continuous coating system by means of DC or MF magnetron sputtering.
  • On the substrate S0, in the exemplary embodiment, float glass with a refractive index of about 1.52, a single base layer GAG with a thickness in the range of 10-40 nm, preferably 15-35 nm is arranged, which serves as a barrier and anti-reflection layer and from a silicon nitride, such as Si 3 N 4 , which has a low aluminum content of a few percent, here preferably in the amount of about eight percent by weight. The base layer GAG of the embodiment has a refractive index of 2.12 ± 0.05. Silicon nitride has also proved to be a suitable barrier layer for the substrate for copper-containing functional layers. The layer is reactively sputtered in the presence of nitrogen as the reactive gas component in the argon working atmosphere from a Si: Al target with 6-10% aluminum content. Alternatively, the layer may also have been deposited without aluminum content and / or under another reactive gas atmosphere or else produced by PECVD.
  • Alternatively, the base layer assembly GA may comprise further layers, e.g. Titanium oxide or niobium oxide, whereby their compared to the base layer GAG higher refractive index and its wavelength dependence would be useful. A seed layer can also be arranged directly below the lower functional layer arrangement UFA. In a further alternative, the base layer GAG is deposited as a substoichiometric layer.
  • Above the base layer arrangement GA, the first, lower functional layer arrangement UFA is deposited. It comprises directly above the base layer GAG a first lower blocking layer UFAB with a thickness of only a few nanometers, preferably less than 1 nm, provided that this blocking layer is not used in addition to the copper layer to further reduce the transmission. Otherwise, the blocking layer may also have higher layer thicknesses, e.g. can be at 2-10nm for chromium nitride. In the described embodiment, in which copper is used for the lower functional layer UFAF, this lower blocking layer UFAB can also be omitted.
  • For a blocker layer different materials come into consideration. Besides the known nickel-chromium used in the embodiment, or stoichiometric or substoichiometric oxide or nitride layers of nickel or nickel chromium, other materials are also usable, e.g. to influence the optical and / or electrical properties of the layer system. For example, e.g. a zirconium oxide layer of various stoichiometry suitable to increase the transmission of the layer system over the use of a nickel-chromium oxide layer and to reduce the sheet resistance of the layer system. A further increase in transmission and reduction in sheet resistance would e.g. with a blocker layer sputtered from a ceramic ZnOx: Al target with 2% aluminum with x <1 without additional oxygen inlet possible. As stated above, titanium oxide TiOx with x ≦ 2 or a niobium oxide layer NbxOy with y / x <2.5 are also possible as a blocking material, the latter also being deposited by the ceramic target without an additional oxygen inlet as substoichiometric layer. Such a deposited layer contains more oxygen than would be achievable with the deposition of a metallic target, resulting in a significantly lower absorption leading to a previously higher transmission associated with a less increase in transmission upon exposure to heat, e.g. as a result of an annealing process.
  • In addition, stoichiometric and substoichiometric chromium nitride, silicon, molybdenum-containing material or stainless steel nitride SST x N y can be used for a blocking layer, these materials also being able to achieve a reduction in the transmission of the layer system in the visible range, for example for use in a low-E-Sun shift system. In this case, the visible transmission decreases with increasing blocker layer thicknesses which deviate from those mentioned above, which can be set even more selectively by using these materials in one or more blocker layers of a layer system comprising one or more functional layer arrangements. In addition, with these materials, the stability of the layer is also opposite Tempering processes, as they are not easily oxidized and not recrystallized at the required low layer thicknesses.
  • Above the lower blocker layer UFAB, the lower functional layer UFAF follows as an IR reflection layer, which in the exemplary embodiment consists of copper and has a thickness in the range of 5-15 nm, preferably 7-13 nm.
  • Alternatively, other copper-containing mixtures or alloys may be used. The copper- or copper-containing layer is sputtered in the DC mode in pure argon atmosphere.
  • Above the lower functional layer UFAF is followed by a further lower blocking layer UFAB made of a nickel chromium oxide with a thickness of only a few nanometers, preferably less than 1 nm. Also for this lower blocking layer UFAB, as described above for the first blocking layer, other materials and layer thicknesses may also be used come.
  • Above the lower functional layer arrangement UFA, an intermediate layer arrangement ZA is deposited. In the exemplary embodiment, it consists of two layers, an intermediate layer ZAZ and a seed layer ZAK deposited over it. The intermediate layer ZAZ consists, in particular because of its particular mechanical stabilizing properties, of an oxide of a zinc stannate with a thickness in the range of 50-85 nm, preferably 60-75 nm. It is obtained from a zinc stannate target which is 50% Zinc and 50% tin, reactively sputtered in the presence of oxygen in the working gas argon. The seed layer ZAK of the intermediate layer arrangement ZA has a thickness of less than or equal to 15 nm, preferably ≦ 10 nm. It consists of a zinc-aluminum oxide sputtered from a Zn: Al target with about 2% aluminum content or from a ceramic zincaluminum oxide target. Alternatively, the layer may also be deposited without aluminum content or a ceramic zinc oxide (so-called intrinsic zinc oxide) target. Alternatively, other materials may be used for one or more of the individual layers as long as they perform the functions described. Alternatively, instead of the one intermediate layer, it is also possible for a plurality of dielectric layers of different composition to be deposited.
  • Above the intermediate layer arrangement ZA, directly adjacent to the seed layer ZAK of the intermediate layer arrangement ZA, an upper functional layer arrangement OFA is deposited which, as described for the lower functional layer arrangement UFA, comprises an upper functional layer OFAF but only an upper blocking layer OFAB above the upper functional layer OFAF. In the exemplary embodiment, the upper blocking layer OFAB corresponds to that of the lower functional layer arrangement UFA, which is likewise arranged above the functional layer, so that reference can be made in this regard to the statements therein. The layer thickness ranges of the upper blocking layer OFAB correspond to those of the lower functional layer arrangement UFA. Alternatively, a blocking layer lying below the functional layer is also possible and other materials can be used for one or more of the individual layers, provided that they fulfill the functions described.
  • The upper functional layer OFAF as an IR reflection layer has a thickness in the range of 10-20 nm, preferably 12-18 nm, and in the exemplary embodiment consists of silver. Alternatively, other silver-containing mixtures or alloys may be used. The silver or silver-containing layer is sputtered in the DC mode in pure argon atmosphere.
  • The IR-reflective layer system is closed at the top by a cover layer arrangement DA. This comprises a first cover layer DA1, which is deposited on the upper blocking layer OFAB. It consists of a low nitrogen oxide or oxynitride of a zinc stannate, has a thickness in the range of 10-20 nm, preferably 12-18 nm, and is under an oxygen-containing or oxygen-containing and nitrogen-containing atmosphere from a zinc stannate target containing 50% zinc and 50% tin, deposited.
  • In the case of a reactive gas composition with a ratio of the volume proportions of nitrogen to oxygen of less than or equal to 0.2, it is entirely possible that, despite a nitrogen content in the reactive gas atmosphere, no nitrogen is incorporated in the first cover layer DA1. This also applies to zinc stannate-containing layers of the intermediate layer arrangement ZA.
  • A second cover layer DA2 of silicon aluminum nitride with a thickness in the range of 10-30 nm, preferably 15-25 nm, is deposited over the first cover layer DA1. This is similar to the base layer GAG of a Si: Al target with 6-10% aluminum content. The refractive index is also comparable to that of the base layer GAG. Alternatively, the layer may also be deposited without aluminum content and / or under another reactive gas atmosphere. In the event that a color correction of the reflection color appearance is required, in which the cover layer is also used, the thickness can also assume values other than those mentioned here.
  • This results in the following composition of the layer system viewed from the substrate S0 upwards:
    GAG Si 3 N 4 with 6-10% Al;
    UFAB NiCr;
    UFAF Cu;
    UFAB NiCrOx;
    ZAZ oxide of a zinc stannate;
    ZAK ZnO with approx. 2% Al;
    OFAF Ag;
    OFAB NiCrOx;
    DA1 oxide or oxynitride of a zinc stannate;
    DA2 Si 3 N 4 with 6-10% Al;
  • A substrate S0 provided with such a layer system as well as an insulating glass unit which uses a pane with this layer system has the desired neutral to slightly blue color appearance of the reflection whose color values of the CIE L * a * b * color system are in the vertical direction of view (viewing direction in 3 represented by three arrows) lie in the claimed areas.
  • In one embodiment, a (triple-low E or triple-low E-Sun) or more (multi-low-E or multi-low E-Sun) functional layer arrangements can be arranged under the cover layer arrangement, each with a further interlayer arrangement are connected to the underlying functional layer arrangement. These further functional layer arrangements may be functional layers containing silver or copper. But other materials with the IR-reflective property, such as. Gold or alloys thereof, a semi-precious metal or tantalum, are usable as far as at least one functional layer contains silver and another copper.
  • The emissivity achieved with the layer system according to the embodiment is less than 3% for a double-low E and less than 2% for a triple-low E.
  • LIST OF REFERENCE NUMBERS
    • S0
      substratum
      GA
      Base layer arrangement
      GAG
      base layer
      UFA
      lower functional layer arrangement
      UFAF
      lower functional layer
      UFAB
      lower blocking layer
      ZA
      Interlayer arrangement
      ZAZ
      interlayer
      ZAK
      seed layer
      OFA
      upper functional layer arrangement
      OFAF
      upper functional layer
      OFAB
      upper blocker layer
      THERE
      overlay assembly
      DA1
      first cover layer
      DA2
      second cover layer
  • QUOTES INCLUDE IN THE DESCRIPTION
  • This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.
  • Cited patent literature
    • DE 03543178 A1 [0012]
    • EP 1174379 A1 [0012]

Claims (8)

  1. Infrared-reflecting, transparent layer system on a transparent substrate (S0) with the following layer arrangements, viewed from the substrate (S0) upward: - a base layer arrangement (GA) with a dielectric base layer (GAG) of a nitride, oxide or oxynitride of a metal, a semiconductor or a semiconductor alloy, a lower functional layer arrangement (UFA) with a metallic lower functional layer (UFAF) for reflection of infrared radiation, at least one intermediate layer arrangement (ZA), which further functional layer arrangement (MFA, OFA) of an underlying functional layer arrangement (UFA, MFA) separates and comprises an intermediate layer (ZAZ, ZAK) or more, - at least one further functional layer arrangement (MFA, OFA) lying above the lower functional layer arrangement (UFA) with a metallic further functional layer (MFAF, OFAF) for reflection of infrared radiation, and - a Cover layer arrangement (DA) with egg ner dielectric, a nitride, oxide or oxynitride of a metal, a semiconductor or a semiconductor alloy containing cover layer (DA1, DA2), characterized in that at least one functional layer copper and at least one functional layer contains silver.
  2. Infrared radiation-reflecting, transparent layer system according to claim 1, characterized in that the lower functional layer contains copper.
  3. Infrared radiation-reflecting, transparent layer system according to claim 2, characterized in that each further above the lower functional layer contains silver.
  4. Infrared radiation-reflecting, transparent layer system according to one of the preceding claims, characterized in that the a * (Rg) and b * (Rg) color values of the CIE L * a * b * color system of the substrate-side reflection in the range of -5 ≤ a * ≤ 1 and -10 ≤ b * ≤ 1 lie.
  5. Infrared radiation-reflecting, transparent layer system according to one of the preceding claims, characterized in that at least one functional layer arrangement (UFA, MFA, OFA) a blocker layer (UFAB) of a metal, a metal mixture or metal alloy or of a substoichiometric or stoichiometric oxide, nitride or oxynitride thereof contains, for protecting the functional layer (UFAF) against oxidation and diffusion processes.
  6. Infrared radiation-reflecting, transparent layer system according to one of the preceding claims, characterized in that at least one functional layer arrangement (UFA, MFA, OFA) under the functional layer (UFAF, MFAF, OFAF) has no blocking layer (UFAB, MFAB, OFAB).
  7. Infrared radiation-reflecting, transparent layer system according to one of claims 5 or 6, characterized in that by means of the number and thickness of the copper-containing functional layers and / or the thicknesses of at least one blocking layer, the transmission of the layer system to values in the range of 25% ≤ Y (T ) ≤ 75% is set.
  8. Method for producing an infrared radiation-reflecting layer system, wherein the layers of the transparent layer arrangements (GA, ZA, DA, UFA, MFA, OFA) of a layer system according to one of the preceding claims are deposited successively on a transparent substrate (S0) by means of vacuum coating.
DE201210207556 2012-05-07 2012-05-07 IR-reflecting, transparent layer system and method for its production Withdrawn DE102012207556A1 (en)

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PCT/EP2013/058077 WO2013167357A1 (en) 2012-05-07 2013-04-18 Transparent ir-reflective layer system and method for producing same

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US4985312A (en) * 1988-12-13 1991-01-15 Central Glass Company, Limited Heat reflecting glass plate with multilayer coating
US5595825A (en) * 1993-09-23 1997-01-21 Saint-Gobain Vitrage Transparent substrate provided with a stack of thin films acting on solar and/or infrared radiation
EP1174379A2 (en) 2000-07-07 2002-01-23 Strapack Corporation Brake structure of a band reel

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US3993845A (en) * 1973-07-30 1976-11-23 Ppg Industries, Inc. Thin films containing metallic copper and silver by replacement without subsequent accelerated oxidation
US6007901A (en) * 1997-12-04 1999-12-28 Cpfilms, Inc. Heat reflecting fenestration products with color corrective and corrosion protective layers
DE102010008518B4 (en) * 2010-02-18 2013-11-28 Von Ardenne Anlagentechnik Gmbh Heat-treatable infrared radiation reflective layer system and method for its production
CN101955324A (en) * 2010-09-29 2011-01-26 吴江南玻华东工程玻璃有限公司 Low emissivity coated glass
CN202379892U (en) * 2012-01-03 2012-08-15 揭阳市宏光镀膜玻璃有限公司 Magnetron sputtering low-cost like-dual-sliver LOW-E glass

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Publication number Priority date Publication date Assignee Title
DE3543178A1 (en) 1985-12-06 1987-06-11 Leybold Heraeus Gmbh & Co Kg A process for the manufacture of disks with a high transmission in the visible spectrum and disks with high reflection characteristics for thermal radiation by the method and prepared
US4985312A (en) * 1988-12-13 1991-01-15 Central Glass Company, Limited Heat reflecting glass plate with multilayer coating
US5595825A (en) * 1993-09-23 1997-01-21 Saint-Gobain Vitrage Transparent substrate provided with a stack of thin films acting on solar and/or infrared radiation
EP1174379A2 (en) 2000-07-07 2002-01-23 Strapack Corporation Brake structure of a band reel

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