EP3903127A1 - Système de couches d'interférence sans substrat de support, procédé pour fabriquer celui-ci et utilisation de celui-ci - Google Patents

Système de couches d'interférence sans substrat de support, procédé pour fabriquer celui-ci et utilisation de celui-ci

Info

Publication number
EP3903127A1
EP3903127A1 EP20705987.4A EP20705987A EP3903127A1 EP 3903127 A1 EP3903127 A1 EP 3903127A1 EP 20705987 A EP20705987 A EP 20705987A EP 3903127 A1 EP3903127 A1 EP 3903127A1
Authority
EP
European Patent Office
Prior art keywords
interference layer
layer system
interference
refractive index
optically transparent
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.)
Pending
Application number
EP20705987.4A
Other languages
German (de)
English (en)
Inventor
Bernhard Von Blanckenhagen
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.)
Carl Zeiss Vision International GmbH
Original Assignee
Carl Zeiss Vision International GmbH
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 Carl Zeiss Vision International GmbH filed Critical Carl Zeiss Vision International GmbH
Publication of EP3903127A1 publication Critical patent/EP3903127A1/fr
Pending legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005—Separation of the coating from the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0026—Activation or excitation of reactive gases outside the coating chamber
    • C23C14/0031—Bombardment of substrates by reactive ion beams
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/44—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by a measurable physical property of the alternating layer or system, e.g. thickness, density, hardness
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
    • G02B5/0825—Multilayer mirrors, i.e. having two or more reflecting layers the reflecting layers comprising dielectric materials only
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
    • G02B5/085—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal

Definitions

  • Interference layer system without a carrier substrate method for producing the same and its use
  • Optical interference layer systems have been known for a long time and are used for a wide variety of purposes. Common to all is optical
  • Interference layer systems that layers are used whose thickness is in the order of magnitude of the wavelength of light.
  • an optical interference layer system is designed for short wavelengths, for example the UV spectral range, or for longer wavelengths, for example the infrared (IR) spectral range, different layer thicknesses result.
  • the optical properties of surfaces for the light can be changed in a defined manner, so that special technical requirements can be implemented.
  • One example is the reduction of the reflectivity of a surface, such an application of an interference layer system also being referred to as an anti-reflective layer or an anti-reflective layer.
  • an interference layer system also being referred to as an anti-reflective layer or an anti-reflective layer.
  • the reflection can be reduced to values below 1% in the visible spectral range.
  • Such anti-reflective coatings are widely used in optical systems in which each lens surface has such an anti-reflective coating. Also found on eyeglass lenses
  • interference layer system is applied to a substrate.
  • Interference layer system many substrates also contribute to the optical imaging of an optical system by acting, for example, as lenses, imaging mirrors, beam splitter plates or beam splitter cubes. With regard to the mode of operation, these substrates are not part of the optical interference layer system, since these substrates are typically thicker than the coherence length of the light used. In general terms, the coherence length of light is the length over which electromagnetic waves are able to interfere. If a layer or a substrate is thicker than this length, this layer or the substrate does not contribute to the optical interference.
  • optical filters which can be selectively adjusted with regard to the spectral range to be filtered or reflected, for example in addition to a reflector effect for the UV-A component Sunlight also have a filter effect into the blue spectral range of visible light or, for example, a selective filter effect for the IR component of sunlight.
  • filters whose dimensions can be reduced in a simple manner. In particular, it is desirable to have such a filter after being crushed
  • next inner layer which in turn envelops the next inner layer, etc.
  • EP 0 950 693 A1 there is the disadvantage that the possibilities for setting the spectral behavior are limited, for example because only a very limited number of layers can be deposited during the production of these pigments.
  • EP 1 270 683 A2 relates to an optical multilayer system based on a
  • US 2002/0171936 A1 relates to a multilayer interference filter in which a central area of the filter is essentially stress-free and unsupported.
  • the filter has a frame surrounding the central area.
  • US 2004/0070833 A1 relates to a Fabry-Perot filter in which a multilayer system is arranged between a first reflector and a second reflector.
  • the object on which the present invention is based is achieved by providing an interference layer system comprising a plurality of optical
  • Interference layer system has no carrier substrate and wherein the optically transparent layers are arranged flat on top of one another, the optically transparent layers from the group consisting of dielectrics, metals and
  • At least one first optically transparent layer has a refractive index m and at least one second optically transparent layer has a refractive index r2 and wherein the first refractive index m and the second refractive index r2 differ by at least 0.1.
  • the reflection curve of the interference layer system has at least two ranges in a wavelength range from 300 nm to 800 nm
  • Interference layer system in which the at least two wavelength ranges of different reflection in a wavelength curve from 300 nm to 800 nm can be freely selected and / or adjusted as required.
  • optical transparent layer or “optically transparent layers” is understood to mean that the layer or layers in the
  • Substantially no light in the visible spectral range preferably no light in the visible spectral range, and / or essentially no radiation in the IR range, preferably no radiation in the IR range, absorbed or absorb. “Essentially no absorption” is understood to mean low absorption.
  • the optically transparent layer (s) is / are preferably transparent to light in the visible spectral range or to radiation in the IR range.
  • the “optically transparent layer (s) is / are essentially transparent only to light in the visible spectral range.
  • the “optically transparent layer (s) is / are essentially transparent only to radiation in the IR range.
  • optically transparent layer or “optically transparent layers” is preferably understood to mean that the materials from which the layer is built up or the layers are built up are preferably only slightly in the visible spectral range , more preferably no, have absorption.
  • the visible spectral range covers a wavelength range from 380 nm to 780 nm.
  • the IR range detects near IR in a wavelength range from 800 nm to 1100 nm.
  • UV-A range covers a wavelength range from 315 nm to 400 nm in the context of the invention.
  • a layer package that consists of the plurality of optically transparent layers preferably has a transmission of more than 20%, preferably at a desired level
  • Wavelength range The transmission of the entire layer package is preferably in a range from 25% to 100%, more preferably from 30% to 98%, more preferably from 40% to 95%, more preferably from 45% to 90%, more preferably from 50% to 85%, more preferably from 55% to 80%, more preferably from 60% to 75%, each in a desired wavelength range.
  • the optical properties of the materials from which the layers are constructed are preferably defined by the refractive index n and more preferably by the absorption index k.
  • Optically transparent layer materials preferably have an absorption index k ⁇ 0.008, more preferably k ⁇ 0.005, more preferably k ⁇ 0.003, more preferably k ⁇ 0.001, in the spectral range which is determined by the respective application.
  • the absorption index is also called
  • Extinction coefficient or called the imaginary part of the complex refractive index.
  • the details of the refractive indices m and n2 and the absorption index k relate consistently to the respective refractive index or absorption index measured at a wavelength of 550 nm.
  • the classic refractive index also called the refractive index or optical density, is an optical material property.
  • the classic refractive index is the ratio of the wavelength of light in a vacuum to the wavelength in the material.
  • the refractive index is dimensionless and generally depends on the frequency of the light.
  • the complex refractive index describes both the temporal and spatial progression of the wave and its absorption.
  • the real-valued component n r which is usually greater than 1, shortens the wavelength in the medium.
  • the complex-valued part dampens the wave.
  • an interference layer system is understood to mean an arrangement of several optically transparent layers in which, when light is irradiated, there is constructive and destructive interference on the individual optically transparent layers due to reflection and transmission phenomena.
  • several optically transparent layers are at least 2, preferably at least 4, more preferably at least 6, more preferably at least 8, more preferably at least 10, more preferably at least 12, more preferably at least 14, more preferably at least 16, particularly preferably at least 18 and very particularly preferably understood at least 20 optically transparent layers. If the absorption index k of at least one optically transparent layer k> 0, preferably k> 0.008, the absorption of incident light also plays a role. The transmission is reduced by absorption.
  • the interference layer system consists exclusively of this arrangement of several optically transparent layers, in which constructive and destructive interference occurs when light is irradiated due to reflection and transmission phenomena on the individual optically transparent layers.
  • the interference layer system is a stack optically transparent layers as specified in claim 1 for generating optical interference.
  • Wavelength ranges, preferably to an extinction of
  • the interference layer system in the context of the invention can also be referred to as an interference filter.
  • the interference layer system of the present invention does not have a carrier substrate.
  • the interference layer system according to the invention therefore does not contain any
  • Platelet-shaped substrates such as glass flakes, SiO 2 flakes, A Os flakes, natural or synthetic mica flakes, etc.
  • Interference layer system have a filter effect for a wavelength range from 360 nm to 450 nm.
  • Interference layer system have a filter effect for certain wavelength ranges of visible light, as specified in Table 1 below.
  • Interference layer system be designed as a heat reflection filter, preferably in the near infrared range.
  • the near infrared (IR) is divided into IR-A in a range from 780 nm to 1.4 gm and IR-B in a range from 1.4 gm to 3 gm.
  • the interference layer system according to the invention preferably has a
  • the interference layer system according to the invention is a heat reflection filter for a wavelength range from 800 to 850 nm.
  • the interference layer system according to the invention is a heat reflection filter for a wavelength range from 850 to 900 nm.
  • the interference layer system according to the invention is a heat reflection filter for a wavelength range from 870 to 950 nm. According to a further preferred embodiment, the interference layer system according to the invention is a heat reflection filter for a wavelength range from 1000 to 1100 nm.
  • the filter properties of the interference layer system according to the invention can be determined by a selection of the materials from which the individual layers of the interference layer system according to the invention
  • Interference layer systems exist whose layer thickness and / or the number of layers and / or their layer sequence are adjusted.
  • the interference layer system according to the invention can, for example, have defined values for the reflection, the transmission and / or the absorption for the light incident on the interference layer system.
  • the filter properties of the interference layer system according to the invention can also be present at certain angles of incidence of the incident light. If the angle of incidence is different from 0 °, the filter properties can also affect the polarized components of the incident light. An angle of 0 ° is understood to mean the case that the light beam hits the surface perpendicularly. If the angle of incidence deviates from 0 °, the angle of incidence to the perpendicular is measured on this surface.
  • the interference layer system according to the invention which has no carrier substrate, can advantageously, with regard to defined filter properties, the
  • the interference layer system according to the present invention is preferably produced by vapor deposition, preferably by means of physical vapor deposition (PVD: physical vapor deposition). It is also possible to produce the individual layers by chemical vapor deposition (CVD: Chemical Vapor Deposition) or by sputtering. According to a preferred embodiment of the invention, the individual layers are applied by means of PVD.
  • the interference layer system of the present invention can therefore also be referred to as an interference layer system generated by vapor deposition, for example as a PVD interference layer system or CVD interference layer system.
  • the interference layer system according to the invention is preferably not
  • the interference layer system according to the invention is a PVD interference layer system.
  • the interference layer system or the interference filter of the present invention can be made film-like or foil-like.
  • the interference layer system can also be used as an interference layer film or as
  • Interference layer film are referred to.
  • the interference layer system can also be embodied in particulate form.
  • the particulate interference layer system has a constant thickness over the entire surface with a maximum deviation of ⁇ 10%, preferably ⁇ 5%, more preferably ⁇ 2%, each based on the total layer thickness of the stack of the individual layers applied one above the other.
  • Interference layer particles have a flat surface. Since the particulate interference layer system is produced by comminution from the interference layer film or the interference layer foil, it preferably has at least partially straight breaking edges. This is done using
  • the interference layer system of the present invention can also be referred to as a UV-A reflector or UV-A interference filter.
  • the interference layer film can therefore also be referred to as a UV-A interference filter film or the interference layer film can also be referred to as a UV-A interference filter film.
  • the interference layer particles can also be referred to as UV-A interference filter particles or UV-A reflector particles.
  • the interference layer system according to the invention can also have a filter effect in the violet and / or blue light range of visible light in addition to a reflector effect in the UV-A range.
  • the interference layer system according to the invention reduces the transmission in the range from 360 nm to 450 nm. According to a further preferred
  • Embodiment of the invention reduces the inventive Interference layer system reduces the transmission in the range from 360 nm to 450 nm by at least 80%.
  • the absorption index k is all
  • Layers of the interference layer system equal to 0 are reflected 80% of the incident light. In practice, a reflection of almost 80% is achieved even if the absorption index k of all layers of the interference layer system is k ⁇ 0.003.
  • the interference layer system of the present invention can also be referred to as a long-pass interference filter.
  • the interference layer film can therefore also be referred to as a long-pass interference filter film or the interference layer film can also be referred to as a long-pass interference filter film.
  • the interference layer particles can also be referred to as long-pass interference filter particles.
  • a long-pass interference filter preferably has a high degree of transmission for long wavelengths and a low degree of transmission for short wavelengths. Long wavelengths are preferably in a range from 420 nm to 780 nm, more preferably from 450 nm to 800 nm.
  • An example of a long-pass interference filter is a UV reflector / olet filter that transmits visible light.
  • the interference layer system of the present invention can also be referred to as a bandpass interference filter.
  • the interference layer film can therefore also be referred to as a bandpass interference filter film or the interference layer film can also be referred to as a bandpass interference filter film.
  • the interference layer particles can also be referred to as bandpass interference filter particles.
  • a bandpass filter preferably has a high degree of transmission for a specific wavelength band, while shorter and longer wavelengths are reflected or absorbed.
  • Such a transmitted wavelength band can for example be in a range from 500 nm to 600 nm, further for example in a range from 540 nm to 580 nm.
  • the transmitted wavelength range can, however, also be different
  • the interference layer system of the present invention can also be referred to as a bandstop interference filter.
  • the interference layer film can therefore also be referred to as a band-stop interference filter film or the interference layer film can also be referred to as a band-stop interference filter film.
  • the interference layer particles can also be referred to as band-stop interference filter particles.
  • a band-stop filter preferably has a low degree of transmission for a certain wavelength range, while shorter and longer wavelengths are allowed through. Such a wavelength range with low transmission can for example be in a range from 500 nm to 600 nm, further for example from 540 nm to 580 nm. The wavelength range with low transmission can, however, also relate to a different wavelength range.
  • the interference layer system of the present invention can also be referred to as an IR interference filter.
  • the interference layer film can also be used as an IR interference filter film or can
  • Interference layer film can also be referred to as an IR interference filter film.
  • the interference layer particles can also be referred to as IR interference filter particles.
  • An IR interference filter preferably has a small one
  • Transmittance for IR radiation in the range from 800 nm to 1100 nm, preferably from 850 nm to 1000 nm.
  • an application medium for example a coating agent
  • Color change or color generation preferably no color change or color generation in the application medium, for example coating agent
  • the interference layer system is designed as a reflector for the UV-A spectral range.
  • the preferably largely colorless or neutral, more preferably colorless or neutral impression enables the interference layer system according to the invention to be used as an optical filter and / or, for example, as a reflector for UV-A light in an application medium, for example a coating agent, without the application medium, for example a coating agent, to change color significantly.
  • the substrate is
  • Interference layer system according to the invention likewise not significantly changed optically, preferably not changed.
  • the interference system according to the invention is used in an application medium, for example a coating agent, there is no color change or color generation in the application medium, for example coating agent, provided the interference layer system is designed as a filter or reflector for the IR spectral range.
  • the interference layer system according to the invention is to be used as a colorant, it can be an application medium, for example a
  • Coating agents for example a lacquer, a paint or printing ink, also impart a coloring, for example blue, green, yellow, red, or combinations thereof.
  • the object on which the invention is based is thus achieved by providing an interference layer system according to claim 1, which preferably also has a reflector and / or filter effect in the UV-A light range and preferably also in the wavelength range from 380 nm to 430 nm, whereby the transmission of the UV-A light through the interference layer system and
  • preferably also in the wavelength range from 380 nm to 430 nm is preferably reduced by more than 25%, more preferably by more than 50%, even more preferably by more than 60%, in each case based on the transmission without the filter effect.
  • the layer thicknesses of the plurality of optically transparent layers in the interference layer system and / or the number of layers can be adjusted to one another depending on the respective refractive index and with regard to the wavelength range to be reflected and / or filtered out.
  • a carrier substrate is understood to mean a substrate to which the optically transparent layers are applied, the substrate usually being mechanically more stable than the optically transparent layers.
  • the interference system can have at least one optically semitransparent metal layer.
  • the interference system of the invention can be constructed exclusively from a plurality of semitransparent metal layers.
  • the metals can be silver, gold, aluminum, chromium, titanium, iron, or alloys, or mixtures thereof.
  • a metal layer is generally semitransparent if the layer thickness is less than 40 nm. Preferably one has
  • Metal layer in the interference layer system according to the invention has a thickness in a range from 5 nm to 38 nm, more preferably from 8 nm to 35 nm, even more preferably from 10 nm to 30 nm, even more preferably from 15 nm to 25 nm. According to a further embodiment of the invention, the
  • Interference layer system both layers which consist of dielectrics, preferably metal oxide (s), and layers which consist of metal (s) on.
  • layers which consist of dielectrics preferably metal oxide (s)
  • metal oxide (s) preferably metal oxide (s)
  • dielectric layers preferably layers of metal oxide (s), and additionally, for example, one, two or three layers
  • Interference layer system also have semitransparent layers which have an absorption index k> 0.001, preferably k> 0.003, preferably k> 0.005, more preferably k> 0.008, for example k> 0.01.
  • This can be, for example, metal oxides at wavelengths that are shorter than the wavelength of the absorption edge.
  • the interference layer system of the present invention is characterized, inter alia, in that there is no carrier substrate for the optically transparent layers.
  • the inventors have found that if the optically transparent layers as such are arranged flat on top of each other and preferably directly flat adjacent to each other, a mechanically surprisingly stable interference layer system is obtained, which in particular can be handled.
  • the interference layer system of the present invention can be designed as a film or foil or also in particulate form. Preferably that exists
  • Interference layer system exclusively from the optically transparent layers arranged flat on top of one another, these each consisting essentially, preferably completely, of one dielectric material or several dielectric materials, preferably one metal oxide or several metal oxides.
  • the interference layer system can be designed in film-like or foil-like fashion with a size of several square centimeters.
  • the interference layer system can for example an area from 1 cm 2 to 400 cm 2 , preferably from 2 cm 2 to 250 cm 2 , more preferably from 4 cm 2 to 150 cm 2 .
  • the interference layer system according to the invention can also have one or more further surface layer (s), i.e. on the outside of the stack of layers of optically transparent layers arranged surface layers, which has / have no optical functions, but improve the application properties.
  • further surface layer i.e. on the outside of the stack of layers of optically transparent layers arranged surface layers, which has / have no optical functions, but improve the application properties.
  • the interference layer system according to the invention can be a
  • Interference layer particles be chemically modified on the surface to one
  • an application medium such as a coating agent.
  • the interference layer system can be flexible so that the film or foil can be rolled up.
  • the interference layer system provided in film or foil form can under
  • interference layer particles or interference filter particles are made available. These particles can have an area of 1 ⁇ m 2 to 1 cm 2 , preferably 5 ⁇ m 2 to 40,000 ⁇ m 2 , more preferably 10 ⁇ m 2 to 10,000 ⁇ m 2 , more preferably 100 ⁇ m 2 to 5,000 ⁇ m 2 .
  • the flat carrier substrate has a low surface roughness, preferably a surface roughness of ⁇ 3 nm rms, more preferably of ⁇ 2 nm rms, further preferably of ⁇ 1 nm rms.
  • Rms is understood to mean the square roughness (rms: root-mean-squared roughness), which is also referred to as R q .
  • the quadratic roughness "rms” or “R q " represents the standard deviation of the distribution of the surface heights, as in ES Gadelmawla et al. , “Roughness Parameters", Journal of Materials Processing Technology 123 (2002) 133-145, section 2.2, the disclosure of which is hereby incorporated by reference.
  • the quadratic roughness R q is defined as specified in formula (II):
  • the optical filter can be a UV reflector, color filter, heat reflection filter or IR filter and / or
  • Application medium from the group consisting of glazes, glasses, plastics, and coating agents, preferably paints, varnishes, printing inks.
  • Application medium a coating agent.
  • the interference layer system according to the invention is distinguished, inter alia, by the fact that it does not have a carrier substrate.
  • the optically transparent layers are arranged flat one above the other and preferably adjacent to one another.
  • “arranged adjacent to one another” is understood to mean that adjacent layers are directly, i.e. are arranged in flat contact with one another.
  • the optically transparent layers are preferably stacked flush in the edge areas. In the interference layer system according to the invention, therefore, in the edge areas, i.e. when viewed "from the side", there are preferably "open layer ends", i.e. not wrapped
  • the optically transparent layers are not applied in an enveloping manner. Rather, it is preferred that the optically transparent layers are defined layer stacks of layers each with a defined layer thickness over the entire width of the interference layer system. With this arrangement of the optically transparent layers, the identical and defined layer sequence, each with a defined layer thickness, is also present in the edge areas as in the middle area of the interference layer system. The edge regions of the optically transparent layers in the layer stack are preferably not encased.
  • the layer thickness of each optically transparent layer is in a thickness range of 5 nm to 500 nm, preferably 6 nm to 460 nm, preferably 7 nm to 420 nm, preferably 8 nm to 380 nm, preferably 9 nm to 320 nm, preferably 10 nm to 280 nm, preferably 11 nm to 220 nm, preferably 12 nm to 180 nm, preferably 13 nm to
  • each layer represents the spatial extent of the layer perpendicular to the surface.
  • the interference layer system according to the present invention can be symmetrical or asymmetrical with regard to the layer sequence
  • An asymmetrical layer structure can result, for example, from the fact that the layer thickness of the layers arranged in the layer stack differs from one another depending on the arrangement in the layer stack.
  • An asymmetrical layer structure can also result from the fact that the metal oxides used in the individual layers are different from one another, so that there is no symmetrical structure.
  • An asymmetrical layer structure can also result from the fact that the two outer layers are on the top and bottom of the
  • Interference layer system are different from each other.
  • the lower surface of the interference layer system can be designed as an SiO2 layer and the upper surface of the interference layer system as a TiO2 layer.
  • none of the optically transparent layers has the function of a carrier substrate.
  • the mechanical stability of the interference layer system according to the invention results from the plurality of optically transparent layers which, viewed individually, usually do not have sufficient mechanical stability.
  • the inventors have surprisingly found that there is sufficient mechanical stabilization of the interference layer system when at least 4, preferably at least 6, more preferably at least 8, more preferably at least 10, more preferably at least 12, more preferably at least 14, optically transparent layers
  • the interference layer system according to the invention is a flat structure which preferably has a total thickness from a range of 40 nm to 5 ⁇ m,
  • the interference layer system comprises 4 to 100, preferably 6 to 80, more preferably 8 to 70, even more preferably 10 to 60, even more preferably 12 to 50, even more preferably 14 to 40, optically transparent layers or consists of it.
  • Interference layer system as a film or foil, preferably as an optical film or optical foil, without a carrier substrate. That in film or foil form
  • the present inventive interference layer system is preferably flexible, so that the interference layer system according to one embodiment of the invention can be rolled up or can be adapted to a substrate.
  • the interference layer system according to the invention can therefore be present as a freely present interference layer film or as a freely present interference layer film or as freely present particles.
  • “free” is understood to mean that the interference layer system according to the invention is in unbound form, i.e. without a carrier substrate or detached from a carrier substrate.
  • Interference layer film can have an area of several square centimeters, for example from 2 to 400 cm 2 , preferably from 3 to 200 cm 2 , more preferably from 4 to 120 cm 2 , even more preferably from 8 to 100 cm 2 .
  • the layer system according to the invention is surprisingly easy to handle, preferably as an interference layer film or interference layer film.
  • the interference layer system present as an interference layer film or interference layer film can be used directly as an optical film, for example in physical examinations or in complex optical systems, for example in
  • Brackets arranged to be used.
  • Interference layer system can be easily comminuted under the action of mechanical forces.
  • inventive means for example, the inventive
  • Interference layer film or the interference layer film according to the invention are comminuted by swirling in a medium, for example a gas or a liquid.
  • the interference layer system according to the invention can also be comminuted by the action of, for example, ultrasound.
  • a defined size distribution can be set depending on the duration and the energy input during the comminution.
  • the interference layer system according to the invention can also have an average particle diameter, also referred to as the average particle size, of, for example, 1 ⁇ m to 500 ⁇ m, more preferably 2 ⁇ m to 400 ⁇ m, more preferably 5 ⁇ m to 250 ⁇ m, even further
  • an average particle size is understood to mean the median value D50 of the volume-averaged size, at which 50% of the particles have a size below the specified D50 value and 50% of the particles have a size above the specified D50 value.
  • the particle size distribution can be determined using laser diffractometry, for example using the CILAS 1064 device.
  • the particles obtained when the interference layer system is comminuted have a uniform, and therefore defined, surface over the entire surface of the particle
  • the interference layer particles are mechanically stable and are essentially flat.
  • the interference layer particles are therefore preferably in the
  • interference layer particles according to the invention in planar form, i.e. not in a rolled up form.
  • transparent layers each have one or more dielectrics, preferably
  • Metal oxide (s) in an amount of 95 to 100% by weight, more preferably 97 to 99.5% by weight, more preferably 98 to 99% by weight, in each case based on the
  • each optically transparent layer it is extremely preferable for each optically transparent layer to consist exclusively of one dielectric, preferably metal oxide, or of several dielectrics, preferably metal oxides. According to a further preferred embodiment, each optically transparent layer consists of a single metal oxide.
  • metal oxide (s) also includes metal oxide hydroxide (s) and metal hydroxide (s) and also mixtures thereof.
  • the metal oxide or metal oxides are extremely preferably pure metal oxide (s) without any water content.
  • the interference layer system according to the invention has at least two low-refractive optically transparent layers with a refractive index m ⁇ 1.8 and at least two high-refractive transparent layers with a refractive index n2.8.
  • the low-index, optically transparent layer has a refractive index m from a range from 1.3 to 1.78 and is preferably selected from the group consisting of silicon oxide,
  • the silicon oxide is preferably SiO2.
  • silicon oxide in particular S1O2, is also understood as a metal oxide.
  • Aluminum oxide is preferably Al2O3 or AlOOH.
  • Boron oxide is preferably B2O3.
  • Magnesium fluoride is preferably MgF2.
  • the low refractive index, optically transparent layer is most preferably selected from the group consisting of silicon oxide, aluminum oxide, magnesium fluoride, and mixtures thereof.
  • the aforementioned low refractive index metal oxides are preferably X-ray amorphous.
  • the silicon oxide is also preferably in the form of S1O2.
  • the aluminum oxide is also preferably in the form of Al2O3.
  • the magnesium fluoride is also preferably in the form of MgF2
  • the high-index, optically transparent layer has a refractive index n2 from a range from 2.0 to 2.9 and is preferably selected from the group consisting of titanium oxide, iron oxide, niobium oxide, tantalum oxide, zirconium oxide, tin oxide, cerium oxide, chromium oxide , Cobalt oxide, and mixtures thereof.
  • the aforementioned high refractive index metal oxides are X-ray amorphous.
  • Titanium oxide is preferably T1O2.
  • the T1O2 is more preferably anatase or rutile, even more preferably rutile.
  • the T1O2 is amorphous, i.
  • the iron oxide is preferably in the form of Fe2O3 (flematite) or Fe3O4 (magnetite), more preferably as Fe203.
  • the niobium oxide is preferably in the form of Nb20s.
  • the tantalum oxide is preferably in the form of Ta20s.
  • the zirconium oxide is preferably in the form of ZrO 2.
  • the tin oxide is preferably in the form of SnO2.
  • the high refractive index layer is selected from the group consisting of rutile, niobium oxide, tantalum oxide, zirconium oxide, and mixtures thereof.
  • the aforementioned high refractive index metal oxides are preferably X-ray amorphous.
  • the titanium oxide is present as T1O2, preferably as rutile.
  • Interference layer system an alternating layer sequence of two optically
  • the first optically transparent layer having a refractive index m and the second optically transparent layer one
  • this includes
  • Interference layer system as a low refractive index layer made of silicon oxide, preferably S1O2, and as a high refractive index layer made from titanium oxide, preferably T1O2, more preferably amorphous T1O2, the
  • Silicon oxide layers and the titanium oxide layers are preferably arranged alternately.
  • Interference layer system in total 4 to 100, preferably 6 to 80,
  • the titanium oxide layers and silicon oxide layers are X-ray amorphous.
  • the interference layer system according to the present invention consists essentially of metal oxide (s), preferably of metal oxide (s). Because of the preferred metal-oxide structure, the interference layer system according to the present invention is not susceptible to corrosion. The application of separate corrosion protection layers is therefore advantageously not necessary. The interference layer system according to the invention is therefore also in one
  • Corrosive environment for example in the presence of water and oxygen, stable to corrosion.
  • the interference layer system according to the present invention is extremely advantageous
  • the invention also relates to the use of an interference layer system according to one of Claims 1 to 16 as an optical filter.
  • the optical filter can be in the form of a film or a foil.
  • the interference layer film or the interference layer film can be arranged in a holder.
  • the present relates
  • an application medium preferably a coating agent, which contains an optical interference layer system according to one of claims 1 to 16.
  • the coating agent can be lacquer, paint or medical products.
  • the application medium can also be a glaze, a ceramic or a plastic.
  • the interference layer system of the present invention can be produced by the method according to claim 17.
  • a flat carrier substrate material is provided which is provided with a separating layer. On this separation layer are then
  • optically transparent layers which are selected from the group consisting of dielectrics, metals, and combinations thereof, to produce an interference layer system according to one of the
  • the flat carrier substrate material can be an inorganic or organic surface.
  • a metallic substrate or a ceramic substrate, for example, can be used as the inorganic surface.
  • a plastic surface can be used.
  • the plastic surface can be modified, for example with a varnish, such as a polysiloxane-based hard varnish.
  • the carrier substrate material can be designed to be immobile, for example as a disk substrate, or mobile, for example as a tape substrate.
  • Carrier substrate material uses a plastic material, as is also used for the production of plastic glasses for glasses.
  • the carrier substrate material can comprise or consist of a plastic material, the plastic material from the group consisting of polythiourethane, polyepisulfide, polymethyl methacrylate, polycarbonate, polyallyl diglycol carbonate, polyacrylate, polyurethane, polyurea, polyamide, polysulfone, polyallyl,
  • the plastic material comprises a polymer material or consists of that from the group consisting of
  • Polythiourethane polyepisulphide, polymethyl methacrylate, polycarbonate,
  • Polysulfone polyallyl, fumaric acid polymer, polystyrene, polymethylacrylate,
  • Biopolymers and mixtures thereof, is selected.
  • the plastic material is most preferably selected from the group consisting of polyurethane, polyurea, polythiourethane, polyepisulfide, polycarbonate, polyallyl diglycol carbonate, and mixtures thereof.
  • Suitable polymer materials are, for example, under the trade names MR6, MR7, MR8, MR10, MR20, MR174, CR39, CR330, CR607, CR630, RAV700, RAV7NG, RAV7AT, RAV710, RAV713, RAV720, TRIVEX, PANLITE, MGC 1.76, RAVolution, etc.
  • the base material of CR39, CR330, CR607, CR630, RAV700, RAV7NG, RAV7AT, RAV710, RAV713 and RAV720 is polyallyl diglycol carbonate.
  • the basic material of RAVolution and TRIVEX is polyurea / polyurethane.
  • the base material of MR6, MR7, MR8 and MR10 is polythiourethane.
  • MGC1.76 is polyepisulphide.
  • plastic materials known from the manufacture of plastic eyeglass lenses are usually provided with anti-reflective and anti-reflective layers, but these are permanently applied to the plastic surface.
  • the carrier substrate is coated with a lacquer, for example a polysiloxane-based hard lacquer.
  • a lacquer for example a polysiloxane-based hard lacquer.
  • a primer layer is arranged between the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer, which the adhesion of the carrier substrate, for example plastic substrate, and the hard lacquer layer
  • the hard paints are typically made using dip coating processes or
  • UV light induces chemical reactions that lead to the hardening of the liquid paint.
  • These hard lacquers are preferably harder than the plastic substrate. These lacquers preferably have an indentation hardness greater than 150 MPa, preferably greater than 250 MPa, measured with the aid of nanoindentation, which is also referred to as an instrumented penetrant test.
  • the instrumented penetration depth is determined, as in Oliver WC and Pharr, GM, "Measurement of hardness and elastic modulus by instrumented indentation: Advances in understanding and refinements to methodology", J. Mater. Res., Vol. 19, No. 1, Jan 2004, pages 3 to 20.
  • the layer thickness of the cured hard lacquer layer is typically 1 ⁇ m, preferably more than 1.5 ⁇ m, for example 2 ⁇ m or 3 ⁇ m.
  • a liquid primer layer is initially preferably applied directly to the plastic substrate
  • this primer layer After this primer layer has been thermally dried, it typically has a layer thickness of> 400 nm, for example from 500 nm to 1 ⁇ m.
  • the primer layer is then preferably applied with a hard lacquer layer, as described above.
  • the primer layer serves to improve the adhesion of the hard lacquer layer to the plastic substrate.
  • the primer for the primer layer is preferably selected from the group consisting of
  • Polyurethane dispersion, polyurethane-polyurea dispersion and mixtures thereof is selected.
  • a commercially available primer is, for example, the primer PR-1165 from SDC TECHNOLOGIES,
  • the hard lacquer is preferably a polysiloxane which, for example, by converting at least one organosilane and at least one tetraalkoxysilane into
  • the cured hard lacquer layer preferably has a roughness ⁇ 3 nm rms, preferably ⁇ 2 nm rms, more preferably ⁇ 1 nm rms.
  • the roughness of the hard lacquer layer can be determined by the choice of solvent,
  • the subsequently applied separating layer as well as that applied to the separating layer are
  • Interference layer system according to the invention is preferably designed as smooth layers which preferably have correspondingly low roughness. In the case of a smooth separating layer and an interference layer system with smooth layers, the interference layer system according to the invention can easily be separated from the
  • interference layer system according to the invention to defined optical
  • Properties for example defined filter properties.
  • a separating layer is applied to the flat carrier substrate material, which separating layer enables the subsequently applied plurality of metal oxide-containing layers to be detached or separated.
  • separating layer Various materials can be used as the separating layer.
  • organic materials can be applied that are soluble in an organic solvent.
  • organic solvent for example, as organic
  • Release agents Waxes or fats that are soluble in organic solvents, for example, can be used.
  • a water-soluble inorganic salt as the separating layer.
  • the use of a water-soluble salt is preferred in terms of work safety and the environment.
  • Salts of the alkali and / or alkaline earth metals are preferably used as inorganic salts.
  • the usual salt formers for example halides, sulfates, phosphates, etc., can be used as anions. To be favoured
  • Halides especially chlorides, are used as anions of the salts.
  • a separating layer made of NaCl is extremely preferred as the inexpensive salt. The separating layer is applied in a suitable layer thickness on the
  • the layer is preferably vapor-deposited onto the flat carrier substrate material with a defined layer thickness in a vacuum.
  • the separating layer thickness can be in a range from 10 nm to 100 nm, preferably from 20 nm to 50 nm.
  • a separating layer thickness of 30 nm, for example made of NaCl, has proven to be very suitable.
  • the separating layer can be applied, for example, with an electron beam evaporator without reactive gas.
  • a defined number of metal oxide-containing layers is then applied to this separating layer in succession and preferably in direct succession by vapor deposition.
  • the number and thickness as well as the nature of the metal oxide-containing layers to be applied depends on the respective
  • Interference layer system set.
  • the separation layer or the plurality of metal oxide-containing layers is applied using a conventional method
  • Vapor deposition system preferably a PVD system (PVD: Physical Vapor Deposition; German: physical vapor deposition).
  • PVD Physical Vapor Deposition
  • German physical vapor deposition
  • Process conditions such as vacuum evaporation rate, inert gas, reactive gas, etc., are set according to the manufacturer's instructions and the desired optical properties of the interference layer system according to the invention.
  • the coating system usually a vacuum coating system, is ventilated.
  • the substrates are then removed and placed in a water vapor-containing
  • Atmosphere stored for example in the ambient atmosphere.
  • the relative humidity is preferably more than 30%.
  • the separating layer for example the NaCl layer, takes from the
  • Ambient atmosphere absorbs moisture and thus reduces the adhesion between the vapor-deposited interference layer system and the flat
  • Carrier substrate material Carrier substrate material.
  • the coating systems from Satisloh GmbH, 35578 Wetzlar, for example the Satisloh 1200-DLX-2, can be used as the coating system.
  • Interference layer systems are produced using the method according to the invention.
  • the calculation of the number and thickness of the layers is computer-based, taking into account the respective refractive index and the desired filter effect. For example, to calculate a
  • transparent optical layer material silicon oxide in particular S1O2, proved.
  • the detached interference layer system preferably an interference layer film or an interference layer film
  • Particle size distribution are comminuted.
  • interference layer system according to the invention can also be incorporated directly into a
  • Coating agents for example a paint or a lacquer
  • Coating agents are introduced and comminuted to a desired particle size or particle size distribution while stirring or irradiating with ultrasound.
  • the interference layer system has a reflection curve which has at least two regions of different reflection in a wavelength range from 300 nm to 800 nm. These at least two areas of different reflection have a defined reflection in the respective wavelength range, the defined reflection of the at least one first reflection area from the defined reflection of an at least second
  • Reflection area is different from each other.
  • a defined reflection can have a fluctuation range of the reflection within the respective range of preferably 25 percentage points, more preferably 20 percentage points, particularly preferably 15 percentage points and very particularly preferably 10 percentage points, each of the maximum reflection value of the respective area.
  • the maximum reflection value does not exceed 100% reflection and the minimum reflection value does not come below 0% reflection.
  • Interference layer system has at least one area in which the reflection for all wavelengths of this area is preferably ⁇ 30%, particularly preferably ⁇ 25% and very particularly preferably ⁇ 20%.
  • the reflection curve of the interference layer system particularly preferably has at least two ranges in which the reflection for all wavelengths of this range is preferably ⁇ 30%, particularly preferably ⁇ 25% and very particularly preferably ⁇ 20 % lies.
  • the reflection curve has a reflection of at least 85%, preferably at least 90% and very particularly preferably at least 95%.
  • the interference layer system has a reflection curve, which for any wavelength lo, preferably selected from a
  • the arbitrary wavelength lo for the first range is preferably to be chosen to be identical to the arbitrary wavelength for the second range.
  • the interference layer system comprises no carrier substrate and at least 4, more preferably at least 6, more preferably at least 8, particularly preferably at least 10 and very particularly preferably at least 12 alternating layers of different refractive indices.
  • the reflection curve of the interference system preferably has at least one wavelength range from 365 nm to 425 nm for each of the mentioned wavelengths a reflection of preferably at least 85%, particularly preferably at least 90% and very particularly at least 95%.
  • the reflection curve has a half width FWHM from a range preferably from 60 nm to 70 nm. Outside the aforementioned wavelength range, in a wavelength range from 440 nm to 800 nm, the reflection curve of the interference system has a reflection of preferably less than 17%, particularly preferably less than 13% and very particularly preferably less than 10%.
  • this comprises
  • Interference layer system at least 20 layers, which alternate
  • lo is a wavelength that can be freely selected, lo is preferably any wavelength in the visible spectral range between 380 nm and 780 nm.
  • the specification of the layer thicknesses in multiples of lo / 4 can be converted into the physical layer thickness d in the unit nm as follows are converted:
  • n the refractive index of the layer at wavelength lo.
  • this comprises
  • Interference layer system at least 22 layers, which alternate
  • this difference in refractive index is preferably at least 0.90, particularly preferably at least 0.952.
  • the relative accuracy for the above calculation of FWHM is 10%.
  • These at least 22 layers preferably include the following optical layer thicknesses according to variant A or according to variant B or according to variant C, where T is one
  • lo is a wavelength which can be freely selected, lo is preferably any wavelength of the visible spectral range between 380 nm and 780 nm.
  • the conversion into the physical layer thickness is carried out as described above
  • this comprises
  • Interference layer system at least 24 layers, which alternate
  • this difference in refractive index is preferably at least 0.90, particularly preferably at least 0.952.
  • lo is preferably identical for both ranges defined above.
  • the relative accuracy for the above calculation of FWHM is 10%.
  • lo is a wavelength that can be freely selected; lo is preferably any wavelength of the visible spectral range between 380 nm and 780 nm.
  • the conversion into the physical layer thickness is carried out as
  • this comprises
  • Interference layer system at least 26 layers, which alternate
  • this difference in refractive index is preferably at least 0.90, particularly preferably at least 0.952.
  • lo is a wavelength which can be freely selected; lo is any wavelength of the visible spectral range between 380 nm and 780 nm.
  • the conversion in the physical layer thickness is as described above.
  • Interference layer systems have a surface roughness of preferably ⁇ 3 nm rms, particularly preferably ⁇ 2 nm rms and very particularly preferably ⁇ 1 nm rms.
  • OptiLayer Software program OptiLayer, version 12.37, from OptiLayer GmbH calculates based on the respective interference system, i.e. of the interference system without a carrier substrate.
  • the interference layer systems described retain their reflective properties, regardless of what is selected as the surrounding medium.
  • the interference layer systems show the same reflection properties in the following surrounding media (optical entry and exit medium) in a range of preferably 10 percentage points, particularly preferably in a range of 5 percentage points of the corresponding areas:
  • interference layer systems can be used both in air and in aqueous and / or oil-based preparations without their
  • the reflection properties of the interference systems can be determined with the reflection spectrometer F10-AR-UV from Filmetrics, Inc., San Diego, CA 92121, USA. This determination can be based on the interference system with
  • the reflection of unpolarized light differs from the reflection of light p- or s-polarized to the plane of incidence. Specifically, the reflection of the unpolarized light is the mean value of the reflection of the p- and s-polarized light. All information on reflection in this application relates to unpolarized light in an angle of incidence range from 0 to 15 °. The optical angle of incidence is determined perpendicular to the surface of the interference layer system.
  • Wavelength range from 300 nm to 800 nm can be chosen variably.
  • the first area and the second area preferably have a different reflection over the respective complete area.
  • the first range and the second range can preferably be set in the wavelength range from 300 nm to 800 nm when designing the interference layer system. This divisibility
  • the wavelength range can be varied so that
  • Reflection curve of the interference layer system for example at least one, preferably exactly one first region with high reflection and at least one second region with low reflection, the at least one first region with high reflection can be in any wavelength range, preferably in any wavelength range from 300 nm to 800 nm, when designing the interference layer system move.
  • Another advantage of the interference layer system described is that its reflection curve is in a first range of at least 60%, more preferably in a first range of at least 65%, particularly preferably in a first range of at least 70% and very particularly preferably in a first range of at least 75% of the half-width FWHM, with
  • This at least one first range preferably this precisely one first range, can be set within a wavelength range of preferably 300 nm to 800 nm when designing the interference layer system, so that the range of high reflection can be variably selected.
  • the at least one area with high reflection and the at least one area with comparatively low reflection can be implemented with a very small number of layers.
  • Interference layer system comprising a plurality of optically transparent layers, the interference layer system not having a carrier substrate and that the optically transparent layers are arranged flat on top of one another, the optically transparent layers being selected from the group consisting of dielectrics, metals and combinations thereof at least one first optically transparent layer having a refractive index m and at least one second optically transparent layer having a refractive index r2 and wherein the first refractive index m and the second refractive index n2 differ by at least 0.1.
  • Clause 2 Interference layer system according to Clause 1, the layer thickness of each optically transparent layer being in a thickness range from 5 nm to 500 nm.
  • Clause 3 Interference layer system according to Clause 1 or 2, the optically transparent layers each having dielectrics, preferably metal oxide (s), in an amount of 95 to 100% by weight, based in each case on the total weight of the respective optically transparent layer.
  • dielectrics preferably metal oxide (s)
  • Clause 4 interference layer system according to one of clauses 1 to 3, the interference layer system having at least 2 low-refractive optically transparent layers with a refractive index m ⁇ 1.8 and at least 2 high-refractive optically transparent layers with a refractive index n2> 1.8.
  • Clause 5 interference layer system according to one of clauses 1 to 4, the interference layer system having or consisting of 4 to 100 optically transparent layers.
  • Clause 6 interference layer system according to one of clauses 1 to 5, the low-refractive-index, optically transparent layer having a refractive index m from a range from 1.3 to 1.78 and preferably from the group consisting of
  • Clause 7 Interference layer system according to one of Clauses 1 to 6, wherein the high-index, optically transparent layer has a refractive index r2 from a range from 2.0 to 2.9 and preferably from the group consisting of
  • Clause 8 Interference layer system according to any one of Clauses 1 to 7, wherein each optical transparent layer consists exclusively of a metal oxide.
  • Clause 9 Interference layer system according to one of Clauses 1 to 8, wherein the low-refractive-index and high-refractive-index optical transparent layers are arranged alternately one above the other and preferably adjacent to one another.
  • Clause 10 The interference layer system according to any one of Clauses 1 to 9, wherein the interference layer system is a foil, a film or a particle.
  • Clause 11 A method of establishing an interference layer system in accordance with any of Clauses 1 to 10, the method comprising the steps of:
  • Clause 12 The method of Clause 11 wherein the optically transparent layers are vapor deposited.
  • Clause 13 The method under Clause 11 or 12 which separates the layer from a water soluble inorganic salt.
  • Clause 14 Optical filter, wherein the optical filter is or contains an interference layer system according to any one of Clauses 1 to 10.
  • Clause 15 application medium, the application medium including an interference layer system according to any one of clauses 1 to 10.
  • Fig. 1 shows a calculated reflection curve of an inventive
  • Interference layer system made up of a total of 26 alternating layers of T1O2 and S1O2.
  • Fig. 2 shows the inventive interference layer film or a
  • Interference layer film according to the invention for which the reflection curve from FIG. 1 was calculated and measured, on a scanning electron microscope slide.
  • Fig. 3 shows an SEM image (SEM: scanning electron microscope) of the
  • interference layer film according to the invention for which the reflection curve from FIG. 1 was calculated and measured and which can be seen in FIG.
  • FIG. 4 shows the reduction in transmission in the wavelength range between 350 nm and 800 nm when using an interference layer system for which the reflection curve from FIG. 1 was calculated and measured and which is shown in FIG.
  • Fig.3 can be seen.
  • Substrate material is a plastic substrate coated with a polysiloxane-based flart varnish MP-1 154D (SDC TECFINOLOGIES, INC.) Arranged as a carrier substrate material in accordance with Fiersteller information.
  • the plastic substrate material was an uncoated spectacle lens made of polymer CR39 which had a circular diameter of 6.5 cm and a thickness in the center of 1.5 mm.
  • the primer PR-1 156 (SDC TECHNOLOGIES, INC.) was first applied to the plastic substrate material in a layer thickness of 750 nm by means of dip coating. The drying took place for 5 min at a temperature of 70 ° C. in a standing oven from Memmert GmbH + Co. KG, D-91 126 Schwabach, type ULE 600.
  • the polysiloxane-based hard lacquer MP-1 154D was then in a layer thickness of 2500 nm applied by means of dip coating. Drying and curing then took place for 120 minutes at a temperature of 110 ° C. in a standing oven from Memmert GmbH + Co. KG D-91 126 Schwabach, type ULE 600.
  • the surface was exposed to ions in a vacuum at a pressure of less than 8 ⁇ 10 4 mbar.
  • the ions came from an End-Hall-type ion source. This ion source is part of the coating system.
  • the ions were Ar ions with an energy between 80 eV and 130 eV. The one that hits the substrates
  • Ion current density was between 20 and 60 pA / cm 2. Ar ions were applied for 2 minutes.
  • Coating system applied at a pressure of 4x10 -4 mbar and with a deposition rate of 0.2 nm / s.
  • a total of 26 layers of T1O2 and S1O2 were then applied in a vacuum at a pressure of 4 ⁇ 10 4 mbar.
  • oxygen was added as a reactive gas (20sccm) so that the layers grew without absorption in the visible spectral range and were therefore optically transparent.
  • the substrate was also exposed to ions. These ions came from an End-Hall-type ion source. This ion source is part of the
  • the ions were oxygen ions with an energy between 80 eV and 130 eV.
  • the ion current density striking the substrates was between 20 and 60 pA / cm 2.
  • the exposure of the growing T1O2 layer with Oxygen ions and the addition of reactive gas contributed to the fact that the T1O2 layers grew as an optically transparent layer.
  • Layers of T1O2 and layers of S1O2 were applied alternately.
  • the first metal oxide layer applied directly to the NaCl separating layer was a TiO2 layer.
  • the respectively applied layer thickness of the TiO2 layer or S1O2 layer is given in [nm] in Table 2.
  • the layer thickness was carried out using an oscillating quartz system (XTC Controller, Inficon, CH-7310 Bad Ragaz), which measures the change in the frequency of an electrical oscillating crystal, the frequency changing with the layer thickness of the growing interference layer system.
  • XTC Controller Inficon, CH-7310 Bad Ragaz
  • the quartz oscillator is in
  • the reflection curve was measured using the F10-AR-UV reflection spectrometer from Filmetrics, Inc. (San Diego, CA 92121, USA) by placing the measuring head, after calibrating the device in accordance with the manufacturer's instructions, on a coated area of the
  • Plastic carrier substrate was placed. This measurement was carried out within 5 minutes of venting the vacuum coating system after the coating had ended. The measurement of the reflection curve was carried out on the interference layer film still adhering to the plastic carrier substrate, since performing the measurement of a reflection curve on an interference layer film detached from the plastic carrier substrate is complex.
  • Interference layer system according to the invention was also present during the measurement via the separating layer, hard lacquer layer and primer layer on the carrier substrate material.
  • a Target reflection curve entered.
  • the software program had algorithms that calculate interference layer systems taking into account boundary conditions.
  • the “gradual evolution” algorithm was selected for the calculation.
  • the substrate material, the primer layer with its optical properties and layer thickness, the hard lacquer layer with its optical properties and layer thickness, the separation layer made of NaCl with its optical properties and layer thickness and the use of T1O2 and S1O2 as layer materials were specified as boundary conditions.
  • the maximum number of layers was limited to 26.
  • the algorithm optimized the number of layers and their thickness until a minimal deviation from the target curve was achieved. As a result of this
  • Target reflection curve The interference layer system detached from the carrier substrate therefore also had the calculated or measured reflection curve.
  • the coated substrates were removed from the coating system and left to stand at room temperature in the laboratory for 5 hours.
  • the relative humidity in the laboratory was more than 30%.
  • the interference layer film or the interference layer film was then pulled off the substrate surface with tweezers.
  • Fig. 3 is an SEM image (SEM: scanning electron microscope) of the
  • interference layer film according to the invention.
  • the individual layers of T1O2 and S1O2 are clearly visible. To get the effect in a more viscous
  • Interference layer film comminuted to obtain interference layer particles.
  • a film of the glycerol containing interference layer particles was then applied to a microscope slide in a layer thickness of 50 ⁇ m, and the spectral transmission in the wavelength range from 350 nm to 1050 nm was measured using an Ultrascan spectrophotometer from Hunter Associates Laboratory, Inc. 11491 Sunset Hills Road Reston, VA 20190-5280, USA.
  • a glycerol film without interference layer particles was measured beforehand.
  • Interference layer particles applied. This was calculated as the difference in the transmission curve with and without interference layer particles in glycerol.
  • Interference layer particles led to a significant reduction in the transmission in a wavelength range ⁇ 430 nm, while the transmission at larger wavelengths was not influenced.
  • the transmission could be further reduced.

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Abstract

L'invention concerne un système de couches d'interférence, comprenant une pluralité de couches optiquement transparentes, le système de couches d'interférence ne présentant pas de substrat de support et les couches optiquement transparentes étant disposées à plat les unes au-dessus des autres, les couches optiquement transparentes étant choisies dans le groupe qui est constitué des diélectriques, des métaux et des combinaisons de ceux-ci, au moins une première couche optiquement transparente présentant un indice de réfraction n1 et au moins une deuxième couche optiquement transparente présentant un indice de réfraction n2 et le premier indice de réfraction n1 et le deuxième indice de réfraction n2 se différenciant d'au moins 0,1. L'invention concerne en outre la fabrication et l'utilisation du système de couches d'interférence.
EP20705987.4A 2019-02-22 2020-02-21 Système de couches d'interférence sans substrat de support, procédé pour fabriquer celui-ci et utilisation de celui-ci Pending EP3903127A1 (fr)

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EP19158947.2A EP3699648A1 (fr) 2019-02-22 2019-02-22 Système de couche d'interférence sans substrat support, son procédé de fabrication et d'utilisation
PCT/EP2020/054698 WO2020169839A1 (fr) 2019-02-22 2020-02-21 Système de couches d'interférence sans substrat de support, procédé pour fabriquer celui-ci et utilisation de celui-ci

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EP20705987.4A Pending EP3903127A1 (fr) 2019-02-22 2020-02-21 Système de couches d'interférence sans substrat de support, procédé pour fabriquer celui-ci et utilisation de celui-ci

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CN113490866A (zh) 2021-10-08

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