EP3713888A1 - Revêtement décoratif doté d'une réflexion augmentée des ir - Google Patents

Revêtement décoratif doté d'une réflexion augmentée des ir

Info

Publication number
EP3713888A1
EP3713888A1 EP18811184.3A EP18811184A EP3713888A1 EP 3713888 A1 EP3713888 A1 EP 3713888A1 EP 18811184 A EP18811184 A EP 18811184A EP 3713888 A1 EP3713888 A1 EP 3713888A1
Authority
EP
European Patent Office
Prior art keywords
glass
coating
ceramic substrate
paste
oxide
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
EP18811184.3A
Other languages
German (de)
English (en)
Inventor
Yvonne Menke-Berg
Vera STEIGENBERGER
Adam O´RYAN
Matthew Moose
Michael Schwall
Stephanie Mangold
Matthias Bockmeyer
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.)
Schott AG
Original Assignee
Schott AG
Schott Gemtron Corp
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 Schott AG, Schott Gemtron Corp filed Critical Schott AG
Publication of EP3713888A1 publication Critical patent/EP3713888A1/fr
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/16—Halogen containing crystalline phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
    • C03C3/115—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
    • C03C3/115—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
    • C03C3/118—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/02—Compositions for glass with special properties for coloured glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/06—Frit compositions, i.e. in a powdered or comminuted form containing halogen
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
    • F24C15/00—Details
    • F24C15/02—Doors specially adapted for stoves or ranges
    • F24C15/04—Doors specially adapted for stoves or ranges with transparent panels
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
    • C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2204/00—Glasses, glazes or enamels with special properties
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2207/00—Compositions specially applicable for the manufacture of vitreous enamels
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/45—Inorganic continuous phases
    • C03C2217/452—Glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/48—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific function
    • C03C2217/485—Pigments
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/34—Masking

Definitions

  • the invention relates to a coating with improved IR reflection as well as a paste and a
  • the invention relates to a
  • oven doors usually have a structure of several, successively arranged glass layers on. To increase the thermal insulation effect, the individual glass panes are spaced apart
  • the heating elements of an electric furnace heat in the form of long-wave, electromagnetic radiation, the heat radiation approximately as
  • Blackbody radiation can be viewed.
  • Wavelength of the radiation emitted by the heating elements is thus dependent on the respective temperature, so that the intensity maximum of the radiation depending on
  • Operating temperature in the range of 1.5 ym to 4.5 ym, in particular in the range of 2.5 ym to 10 ym may be.
  • the disadvantage here is the relatively high cost of the conductive oxides.
  • Indium tin oxide, fluorine-tin oxide, aluminum-zinc oxide and antimony-tin oxide do not show high scratch resistance or resistance.
  • the reflection behavior of the corresponding oxides is often optimized for heat radiation in the area of solar heat radiation, since such layers were also borrowed from building glazings.
  • the outer disk i. the disc that forms the outside of the oven door is usually additionally with a
  • This decorative layer is usually applied as enamel or glass flow layer and preferably contains black, brown and / or white Pimente.
  • the decorative layer is applied mostly in the form of grid or dot matrix on the disc.
  • the patent application WO 2017/216483 A1 describes a coated flat glass with a multilayer coating comprising a layer with a transparent, conductive oxide and a black layer deposited thereon
  • Enamel layer as a decorative layer. This covers the
  • Enamel layer 10 to 60% of the flat glass surface The particle size of those in the enamel layer Pigment particle is in the range of 500 nm to 10 ym and thus in the wavelength range of the heat radiation, so that the corresponding electromagnetic radiation to the
  • Pigment particles can be scattered.
  • the large particle size is disadvantageous in view of the processability of the pigments.
  • corresponding enamel coatings are usually applied by screen printing on the substrate.
  • screens with a correspondingly lower thread density can be used, which in turn can significantly limit the resolution of the printed decoration.
  • the pigment layer serves to enable an improved tempering process, essentially by virtue of the fact that far-infrared wavelengths which correspond to a temperature of more than 600 ° C, nor to
  • Heating the glass can be used and thus to an improved thermal curing of the glass including the double layer containing the conductive pigments
  • Another way of reducing heat loss known in the art is to provide the furnace doors with reflective metal bands, such as silver or aluminum bands, thus directing the heat radiation back into the interior of the furnace.
  • the door design can also have forced convection cooling.
  • Another object of the invention is to provide an oven door or
  • the invention relates to a paste for producing an IR-reflecting layer, in particular on a glass or glass-ceramic substrate, comprising at least one IR-reflecting pigment and glass powder.
  • an IR-reflecting pigment is in particular a
  • Understood pigment having a remission of at least 50% at a wavelength of 1500 nm. Due to the high remission of the infrared (IR) radiation, a large part of the heat radiation is thus remitted or Remission was determined according to the standard ISO 134 68.
  • IR infrared
  • the pigment has a TSR of at least 20%.
  • the TSR value total solar reflectance
  • the TSR value provides information on the percentage of reflected electromagnetic radiation in the wavelength range from 200 nm to 2500 nm and is determined in accordance with the ASTM G 173 measurement standards.
  • Thermal radiation influenced.
  • a high TSR value is advantageous in order to achieve a high remission of the heat radiation, i. from electromagnetic radiation in the range of 1 to 4 ym. This is surprising insofar as the wavelength ranges of heat radiation and the
  • Wavelength range which is relevant for the determination of the TSR value, only partially overlap.
  • the TSR value as the transmission value for the solar radiation also refers to the wavelength range of 200 nm to 1000 nm, and thus to much lower
  • the paste at least one IR-reflecting pigment has a TSR value of at least 25%.
  • the pigment at a wavelength of 1500 nm has a reflectance measured according to ISO 13468 of at least 60% or even at least 70%.
  • the particles of the IR-reflecting pigment have a size distribution with a d50 value in the range from 0.5 ⁇ m to 2 ⁇ m. The small particle size makes it possible to apply the paste even with close-meshed screens, for example sieves with a thread count of 77 threads / cm or even 100 threads / cm, so that coatings or decors with high graphic resolution can be produced by screen printing , In the table below are
  • the IR-reflecting pigments have a particle size distribution with a d 50 value in the range from 0.8 ⁇ m to 1.8 ⁇ m.
  • Wavelengths are each assumed to be in the form of black body radiation, in which the emitted spectrum is defined by indication of the temperature.
  • Black body radiators are associated with high accuracy.
  • the paste comprises a chromium-containing IR-reflecting pigment, preferably a chromium-containing iron oxide, a chromium-containing hematite and / or a chromium iron nickel spinel.
  • the IR-reflecting pigment preferably has a black or black-brown color.
  • the respective pigments have a high thermal stability and a high chemical inertness to the glass components of the glass powder in the paste, in view of the penetration of the paste for producing the corresponding enamel coating
  • Embodiment the possible maximum penetration temperature not limited by the stability of the pigments. This allows in a development of the invention the
  • Glass substrate can be thermally biased.
  • the glass powder contained in the paste has a
  • the glass in the paste preferably contains zinc oxide and / or bismuth oxide. Glass powder which has a content of zinc oxide in the range from 0.1 to 70% by weight and in particular one has proved to be particularly advantageous
  • Zinc oxide content in the range of 0.1 to 30 wt .-% have.
  • the glass powder contains 0.1 to 75 wt .-% and in particular 8 to 75 wt .-% bismuth oxide.
  • Softening temperatures in the range of 500 to 950 ° C.
  • the softening temperature is less than 800 ° C, or even less than 750 ° C, and more preferably less than 680 ° C, but more than 450 ° C on. Due to the low softening temperatures already at low Einbrandtemperaturen the formation of a
  • the content of bismuth oxide in the glass will correspond to the chemical resistance, i. the coating made with the paste increases.
  • the glass matrix or the glass flux in the coating of the coated substrate has the same composition as the glass powder in the paste, the
  • B2O3 0-30 preferably 1-30, particularly preferably 5-30
  • Na 2 0 0-25 prefers 0-15
  • the glass preferably has a minimum content of Al 2 O 3 of 0.2% by weight, preferably of at least 2% by weight.
  • the glass has a content of B 2 O 3 of at least 1% by weight, preferably at least 5% by weight.
  • the glass contains at least 1% by weight of an alkali metal oxide chosen from the group of Na 2 O, Li 2 O and K 2 O or mixtures of these oxides.
  • the glass comprises at least 1% by weight of a further oxide or a mixture of oxides selected from the group of CaO, MgO, BaO, SrO, ZnO,
  • the glass has the following composition in% by weight:
  • Si0 2 6-65 preferably 10-65, more preferably 15-65
  • the glass has a minimum content of Si0 2 of 10 wt .-%, preferably of at least 15 wt .-%.
  • the glass has a minimum content of Bi 2 O 3 of 5% by weight, preferably of at least 10% by weight.
  • the glass contains at least 1% by weight, preferably at least 3% by weight, of B 2 O 3 .
  • the total content of the alkali oxides Na 2Ü , Li 2 0 and K 2 O is at least 1 wt .-%.
  • the glass contained in the paste or the glass flux in the corresponding coating can in particular
  • alkali-free glass an alkali containing glass, a silicate glass, a borosilicate glass, a zinc silicate glass
  • Zinc borate glass a zinc borosilicate glass, a
  • Bismuth borosilicate glass a bismuth borate glass, a
  • the paste has glass powder with different
  • Paste in particular of conductive oxides selected from the group consisting of the elements indium-tin oxide, fluorine-tin-oxide, aluminum-zinc-oxide and antimony-tin-oxide less than 500 ppm.
  • conductive oxides selected from the group consisting of the elements indium-tin oxide, fluorine-tin-oxide, aluminum-zinc-oxide and antimony-tin-oxide less than 500 ppm.
  • none of the abovementioned oxides are added to the paste.
  • the paste comprises 10 to 40% by weight of IR-reflecting pigments, 45 to 85% by weight of glass powder and 12 to 35% by weight of screen printing medium.
  • solvents for screen-printable coating solutions preference is given to using solvents having a vapor pressure of less than 10 bar, in particular less than 5 bar and very particularly less than 1 bar.
  • solvents having a vapor pressure of less than 10 bar in particular less than 5 bar and very particularly less than 1 bar.
  • These may be, for example, combinations of water, n-butanol, diethylene glycol monoethyl ether, Tripropylene glycol monomethyl ether, terpineol, n-butyl acetate.
  • organic additives may include hydroxyethyl cellulose and / or hydroxypropyl cellulose and / or
  • Block copolymers and / or triblock copolymers and / or tree resins and / or polyacrylates and / or polymethacrylates are examples of screen printing oils.
  • screen printing oils for example, the oils listed in the table below can be used:
  • composition of the paste described above ensures that a coating produced therefrom has a high IR reflectivity.
  • proportion of the screen-printing medium ensures good processability of the paste, in particular processing by means of
  • the paste preferably has a viscosity in the range of 3.5 Pa * s at a shear rate of 200 / s to 15 Pa * s at a shear rate of 200 / s, more preferably in the range of 4.8 Pa * s in one
  • the paste has a means which under temperature increase below
  • Formation of a volatile phase decomposes.
  • such agents are included which split off gas.
  • the means are designed so that their dimensions
  • Anions in the temperature range of the viscous melt of the glass flux gas form and the cations of the agent without affecting the desired properties in the Glass matrix are involved.
  • Such agents are also referred to as blowing agents or foaming agents.
  • blowing agents are agents which contain carbides, carbonates or bicarbonates and
  • Manganese compounds include. Also, substances which are formed as hydroxides and / or water of crystallization
  • this includes salts, clay minerals, borates or aluminates. Phosphates or sulfates are also suitable as blowing agents.
  • Phosphates or sulfates are also suitable as blowing agents.
  • Blowing agents can be used alone or in mixtures.
  • organic substances can also be used as blowing agents.
  • this includes substances which decompose at the temperatures considered here to form gas, in particular tartrates such as potassium bicarbonate, but also sugar or wood dust.
  • blowing agents comprising starch.
  • rice starch, corn starch and potato starch are particularly suitable as blowing agents.
  • Certain oxides decompose with elimination of a gas, such as cerium (IV) oxide or manganese (IV) oxide.
  • a swelling or foaming agent is understood as meaning those agents which are found in
  • Cooling of the coated substrate may be at room temperature in another state of aggregation. If, for example, decomposition temperature from a
  • Blowing agent forms water vapor as a volatile substance, it may be that after cooling of the coated substrate in the pore not more water vapor, but liquid water is present.
  • Zerset Z non-volatile substance at room temperature is present as a condensate.
  • the spatial configuration or the shape of the pores can be influenced by the particular blowing agent used.
  • the paste contains calcium carbonate as a blowing agent.
  • the resulting pores when the paste is burnt in have symmetrical or at least substantially symmetrical structures, with the pores largely are spherical and a round or
  • Another embodiment provides for the use of rice starch as a blowing agent.
  • rice starch as a blowing agent.
  • Embodiment obtained porous enamel has pores with an anisotropic pore structure.
  • the pores in particular have an ellipsoidal cross-section.
  • the coatings include fully closed pores of the present invention Revelation some IR reflection in the form
  • a lowering of the temperature of one side, in particular the uncoated front of a window (the oven interior facing away from the oven inside, or the side facing away from the fireplace, the fireplace), for example, a oven door, or a window in a fireplace or a Furnace, in comparison to a coating which comprises no pores or only very few pores, in particular no or only very few closed pores, is present.
  • Component of the paste can be found in the following table.
  • the pastes for producing a porous, IR-reflecting coating contain a proportion of blowing agent in the range from 5 to 30% by volume, preferably from 5 to 15% by volume. Blähschanteile in this area have been found to be particularly advantageous in terms of the IR reflectivity of the resulting paste. It can be assumed here that structural elements are present through the interfaces of the pores in the coating, by means of which the IR reflectivity, for example by scattering effect, is increased. It can be assumed that these scattering effects occur especially in coatings with closed pores. However, high levels of blowing agents in the paste can cause open pores to form.
  • a development of the invention provides that the paste contains at least one further, second IR-reflecting pigment. Preference is given to the second IR-reflecting Pigment selected from the group of elements
  • Cobalt titanate spinel Preferably, the proportion of the second IR-reflecting pigment in the paste 0.5 to 15 wt .-%, preferably 3.5 to 12.5 wt .-%.
  • the volume ratio between the volume of the second pigment and the volume of the first pigment is 0.03 to 0.6, preferably 0.05 to 0.56 and particularly preferably 0.14 to 0.47.
  • the invention relates to a glass or
  • a glass-ceramic substrate comprising a surface area with a coating. Under a coating will
  • a surface region understood, which comprises a superficial diffusion of the coating in the near-surface regions of the substrate.
  • Coating may thus also include diffusion layers at the boundary between the coating and the substrate.
  • the coating contains a glass matrix and an IR-reflecting pigment, with the IR-reflective
  • Pigment has a TSR value of at least 20% measured according to the standard ASTM G173.
  • the coating exhibits a reflectance of at least 35% measured at a wavelength of 1500 nm, in accordance with the measurement standard ISO 13468.
  • TSR value refers to the solar spectrum with substantially smaller wavelengths in the range from 200 nm to 1000 nm.
  • the pigment has a TSR of at least 25%.
  • the pigments are homogeneously distributed in the glass matrix, hereinafter also referred to as glass flow.
  • the pigments have a
  • the pigments thus have a particle size which is below the wavelength of the heat radiation to be reflected.
  • the layer still shows a high remission for radiation in the IR range.
  • the layers according to the invention have a remission of at least 35% at a wavelength of 1500 nm.
  • the remission at 1500 nm is at least 40% or even at least 45%.
  • Coating is 15 to 45 wt .-%, preferably 15 to 35 wt .-%.
  • a corresponding pigment content ensures a sufficient IR remission of the coating. simultaneously the pigment content is small enough to be homogeneous
  • the proportion of the glass matrix in the coating is preferably 55 to 85% by weight.
  • the coating therefore preferably has a layer thickness in the range from 8 to 35 ⁇ m, preferably 10 to 20 ⁇ m. The coating is thus thick enough to allow a sufficiently high remission of the IR radiation
  • the coating can be used independently of the CTE of the substrate.
  • the use of chromium-containing pigments as IR-reflecting pigment has proven to be particularly advantageous.
  • the coating preferably comprises, as the IR-reflecting pigment, a chromium-containing iron oxide, a chromium-containing hematite and / or a chromium iron comprising nickel spinel.
  • the temperature stability of the pigments is not only for the use of the coated substrate,
  • the IR-reflecting pigment preferably has a black or black-brown color.
  • the IR-reflecting pigment is selected from the group comprising the elements of the pigments Ci Brown 29, Ci Green 17 and Black CI 7.
  • the coating has at least a first and an IR-reflecting pigment.
  • the color location of the coating can be adjusted by the second IR-reflecting pigment.
  • the coating preferably contains, as the second IR-reflecting pigment, a cobalt chromite spinel, an indium manganittrium oxide, a niobium sulfur oxide, a tin zinc titanate and / or a cobalt titanate spinel.
  • the use of one of the pigments from the group having the elements C. Pigment Blue 36, CI Pigment Blue 86, CI Pigment Yellow 227, CI Pigment Yellow 216, CI Pigment Green 26 and CI Pigment Green 50 has proven to be particularly advantageous.
  • the proportion of the second IR-reflecting pigment in the coating is preferably 0.75 to 18.5
  • Wt .-% particularly preferably 4.5 and 14 wt .-%.
  • the volume ratio between the volume of the second pigment and the volume of the first pigment is 0.03 to 0.6, preferably 0.05 to 0.56 and particularly preferably 0.14 to 0.47.
  • the content of conductive oxides in the coating is less than 500 ppm.
  • conductive oxides are in particular transparent conductive oxides (TCO,
  • Transparent conductive oxides such as
  • Indium tin oxide, fluorine-tin oxide, aluminum-zinc oxide and antimony tin oxide understood.
  • the coating is applied directly to the substrate surface.
  • the glass or glass-ceramic substrate does not have a conductive oxide coating.
  • no coatings comprising conductive oxides are arranged on the coating according to the invention and / or between the coating according to the invention and the glass or glass-ceramic substrate.
  • a development of the invention provides that the applied to the glass or glass ceramic substrate
  • Coating comprising closed pores.
  • the suspension or paste comprises the present
  • Coating the present development therefore, according to an embodiment also be designed as foam enamel.
  • the coating is hereby used as a barrier to the passage of fluids, e.g. Water or too
  • Fluids in the sense of the present disclosure preferably comprise liquids, in particular water, aqueous liquids, alcohols, on these liquids
  • Liquids such as window cleaners, and / or oils and water vapor.
  • the coating is a high temperature stable
  • a high-temperature-stable coating is understood in particular to mean a coating which is stable to temperatures of more than 400 ° C.
  • a coating is referred to as self-sealing if no further coating is necessary in order to prevent sufficient sealing against the entry or passage of fluids.
  • the layer thus has a barrier effect against fluids.
  • Embodiments of the present invention is thus self-sealing, for example as a barrier to the passage of fluids formed.
  • the porous coating is inorganic.
  • the coating can also contain organic substances
  • the coating is substantially inorganic. Essentially inorganic here means that the
  • Coating comprises at least 95% by weight of inorganic constituents, preferably at least 98% by weight of inorganic compounds
  • An embodiment provides that the resulting coefficient of thermal expansion of the porous coating and the coefficient of thermal expansion of the substrate differ from each other by not more than 4 * 10 6 / K in the temperature range from 20 ° C to 700 ° C.
  • Expansion coefficient includes, in particular one
  • Coefficient of expansion of the coating a value between at most 9 * 10 -6 / K and at least 3 * 10 -6 / K on.
  • the substrate comprises a soda-lime glass or a borosilicate glass.
  • the glass is thermally toughened to increase strength.
  • a development of the invention provides that the
  • Coating has a refractive index n d, coating in the range of 1.3 to 2, preferably in the range of 1.5 to 1.8
  • a preferred embodiment of the invention provides that the coating is applied laterally structured on at least one surface of the glass or glass-ceramic substrate. This is under a lateral
  • Structuring in particular understood that only parts of the substrate surface are coated.
  • at least 60%, preferably at least 62%, and most preferably at least 65%, are at least respective ones
  • Substrate surface coated with the coating The high degree of occupancy of the substrate surface with the coating.
  • Coating ensures a high IR reflection averaged over the entire substrate surface.
  • grid-shaped pattern of the coating allows it Here, to achieve high occupancy levels while maintaining the transparency through the substrate.
  • the invention further relates to household appliances,
  • One aspect of the invention in this case regards a baking-oven door with a pane construction with at least two panes, wherein the substrate coated according to the invention is used as an outer pane.
  • the outer pane is understood to be the pane of the oven door which is in contact with the space surrounding the oven.
  • the substrate is a glass substrate and on one side with the
  • Glass substrate in this case points in the direction of the furnace interior and at least 60%, preferably at least 62%, particularly preferably at least 65% and very particularly preferably at least 70% of the surface of the glass substrate are covered with the coating.
  • the glass substrate preferably has an occupancy rate of at least 60%.
  • the heat loss can be significantly minimized by thermal radiation, so that depending on the application to further measures to reduce the heating of the outer
  • the outer disc can be dispensed with.
  • the outer disc has no further
  • Coating comprising a conductive oxide.
  • Baking oven door comprises at least three glass panes and the outer and the middle glass pane are formed as inventively coated glass substrate.
  • the middle glass pane is provided on both sides with the coating according to the invention.
  • the invention relates to a method for
  • Production of a glass or glass-ceramic substrate comprising a surface area with a glass matrix and IR-reflecting pigments, in particular for producing a glass or glass-ceramic substrate according to one of claims 15 to 33, comprising at least the following steps: a) providing a glass or glass substrate
  • Step b) provided on the provided in step a) glass or
  • a preferred variant of the method provides that in step a) a glass substrate, preferably a soda lime glass or a borosilicate glass is provided and the
  • step d) the burn-in and the thermal pre-stressing are carried out at a temperature in the range of 500 to 1000 ° C.
  • a crystallizable green glass is provided as substrate in step a).
  • step d) a ceramization of the substrate take place simultaneously with the penetration of the layer.
  • the coating thus obtained is provided with pores in such a way that a coating, which is formed as a barrier to the passage of fluids, is present.
  • the method comprises the following steps: a. Preparation of a suspension or paste.
  • the suspension comprises a glass powder and an agent which decomposes upon raising the temperature to form a volatile substance.
  • blowing agents comprising carbonates and / or phosphates, in particular at layer thicknesses of the coating between 0.1 .mu.m and 500 .mu.m.
  • the glass powder is selected by way of example from the following composition range in% by weight:
  • the glass here advantageously comprises a minimum content of Al 2 C> 3 of 1 wt .-%, preferably of at least 2 wt .-%.
  • the glass comprises at least 1 wt .-% B 2 0 3 , preferably at least 5 wt .-%. According to yet another advantageous
  • the glass comprises at least 1 wt .-% of an alkali metal oxide selected from the group of Na 2 0, Li 2 0 and K 2 0 or mixtures of these oxides.
  • the glass comprises at least 1% by weight of a further oxide or a mixture of oxides selected from the group of CaO, MgO, BaO, SrO, ZnO, ZrO 2 , and TiO 2 .
  • the glass is selected from the following composition range in% by weight:
  • the glass flux may further be selected from the following types of glasses: alkali-free glasses, alkaline glasses, silicate glasses, borosilicate glasses, zinc silicate glasses, zinc borate glasses, zinc borosilicate glasses,
  • Bismuth silicate glasses phosphate glasses, zinc phosphate glasses, aluminosilicate glasses or lithium aluminosilicate glasses.
  • the glass powder comprises mixtures of different glasses.
  • the suspending agent is formed as a liquid and may for example comprise water.
  • the suspending agent comprises solvents, for example organic solvents.
  • the solvents preferably have a vapor pressure of less than 10 bar, preferably less than 5 bar, and more preferably less than 1 bar. This includes, for example, water, 2- (2-butoxyethoxy) ethanol, 2-methoxy-methylethoxy-propanol, 2-butoxy-ethanol, n-butanol,
  • additives which may be inorganic or organic
  • Organic additives include, for example, hydroxyethyl cellulose and / or hydroxypropyl cellulose and / or xanthan and / or
  • Triblock copolymers and / or tree resins and / or polyacrylates and / or polymethacrylates are Triblock copolymers and / or tree resins and / or polyacrylates and / or polymethacrylates.
  • the homogenization of the mixture takes place in a next step, for example in a three-roll chair.
  • this powder for example comprising a glass powder, a blowing agent and a pigment, and to homogenize this mixture, for example in a tumbler. Subsequently, this powder can then be pasted as described above.
  • the suspension preferably has a viscosity at a shear rate of 200 / s, measured with a cone plate viscometer, between 2,000 mPas and 20,000 mPas, preferably between 2,500 mPas and 15,000 mPas, particularly preferably between 3,000 mPas and 10,000 mPas. a. Apply the suspension to a substrate so that
  • the suspension or paste to the substrate can take place over the entire surface, although it is also possible for the suspension to be applied in the form of specific patterns , For example, in this way patterns or
  • Font Z oak or other raster are applied to the substrate.
  • Particularly preferred application methods include ink-jet printing, offset printing, pad printing, wet decals,
  • Spray coating, knife coating, flooding and spin coating b. preferably fixing the suspension applied in step b to the substrate, preferably at a temperature between 0 ° C and 300 ° C.
  • step b After at least partial in step b
  • suspension to the substrate is preferably carried out fixing the suspension on the substrate.
  • This can be done for example by a drying step at elevated temperatures, for example at a temperature between 0 ° C and 300 ° C.
  • the fixing of the suspension on the substrate is particularly advantageous if, after the successful application of the suspension to the substrate, it has to be transported to another process unit,
  • composition of the suspension have as preferred areas for fixing a
  • Substrate at a temperature between 500 ° C and 900 ° C, so that the blowing agent decomposes to form at least one volatile substance and in the coating closed pores are formed.
  • the annealing is carried out at a temperature between 500 ° C and 900 ° C.
  • predetermined pattern on the substrate such as a glass or glass ceramic substrate applied.
  • the application of the suspension is advantageously carried out by means of a printing process, for example by means of ink-jet printing, offset printing, pad printing or screen printing, or by means of rolling, flooding, dipping, spraying, knife coating or spin coating.
  • Fig. 1 is a schematic representation of a
  • Fig. 2 is a schematic representation of a coated
  • Fig. 3 is a graphical representation of total
  • Fig. 5 is the graphical representation of
  • Color locus of the coating depends on the coating omposition Z,
  • Fig. 6-8 are schematic representations for the construction of a
  • FIG. 9 is a schematic representation of the outer pane of a oven door with different degrees of occupancy
  • Fig. 14 is a schematic representation of the measuring structure for
  • Determination of the surface temperature of the outer oven disk By setting different temperatures, a pyrolysis operation at 468 ° C (875 ° F) or baking at 246 ° C (475 ° F) can be simulated. 15 is a schematic representation of the measuring structure for determining the surface temperature of the outer oven pane during the simulation of a baking process at 450 ° C,
  • Embodiment and the comparative example at an operating temperature of the oven of 475 ° F (246 ° C),
  • Fig. 17 is a graphic representation of the
  • Embodiment and the comparative example at an operating temperature of the furnace of 875 ° F (468 ° C),
  • Fig. 18 is a graphical representation of
  • Fig. 19 is a graphical representation of the in-line
  • Fig. 20 is a diagram of a schematic
  • 21 is a graphical representation of a porous enamel coated substrate as another embodiment, wherein the porous enamel has largely anisotropic pores.
  • Fig. 22 is a graph of the measured
  • Embodiments which differ in terms of the porosity of the coating at an operating temperature of the furnace of 450 ° C and
  • FIG. 23 shows a representation of the averaged values of in
  • Fig. 22 shown temperature curves
  • Fig. 24 is a graph of the measured
  • Fig. 1 shows the schematic representation of a
  • the coating 2 is applied to one of the surfaces of the substrate 1, while the other surface 110 of the substrate 1 is uncoated.
  • the coating 2 is in this case laterally structured on the surface region of the substrate 1 shown in FIG. 1, so that substrate 1 also has uncoated regions 120 on the coated surface 100.
  • the Coating 2 can be applied, for example, in the form of a grid or in the form of a dot matrix.
  • the degree of coverage of the substrate is understood to mean the ratio of the coated surface to the entire surface 100.
  • Fig. 2 shows the schematic representation of a
  • the substrate 1 is provided over its entire surface with a coating 3, which contains conductive oxides, such as indium tin oxide.
  • the coating 3 thus represents the IR-reflecting layer in the comparative example.
  • a pigmented decorative layer 4 is also applied to the layer 3. in the
  • layer 4 is merely a decorative layer.
  • Substrate is first a paste comprising an IR-reflecting pigment, a glass powder and a
  • Table 1 lists various IR-reflecting pigments which are known as
  • Coating glass component can have very different compositions. There are many
  • Glass compositions are known which, adapted to the deformation temperature of the substrate to be coated, a softening range of about 500 ° C to 1000 ° C.
  • Table 2 shows some glass compositions
  • the glass powders listed in Table 2 have proven to be particularly advantageous in terms of
  • the softening temperature (T E w, ci aspuiver) of the glass relevant because for the smooth flow, ie for
  • the penetration temperature must be at least the
  • Softening temperature Ew of the glass powder correspond.
  • the softening temperature Ew is the temperature at which the viscosity of the glass is 10 7 ' 6 dPas. Depending on the disc geometry and the heating process will be
  • Example 9 is a
  • the transmission is the total transmission measured according to the ASTM D1003 standard.
  • the curve 60 corresponds to the embodiment 1, the curve 61 of the embodiment 2, curve 62 of the embodiment 3 and curve 63 of the embodiment 4.
  • Curve 5 represents the transmission of Comparative Sample 9 and was applied with a 43 mesh / cm mesh screen. Here lies the layer thickness over the
  • Embodiments especially in the longer wavelength range of 1500 nm below the transmission of the comparative example. It should be noted that the
  • Comparative example will be even more pronounced for layers of the same layer thicknesses.
  • the IR-reflecting pigment used has a greater influence on the transmission as the glass composition of the glass matrix.
  • the layers of the transmission curves 60 and 61 differ in their glass composition, but have the same pigment.
  • the samples 60 and 62 have the same glass composition, but differ by the pigment used.
  • FIG. 4 shows the wavelength characteristic of the remission of samples 7 and 8 as well as comparative example 9 from table 3.
  • the remission process shown in FIG. 4 is the total remission measured according to measurement standard ISO 13468.
  • Samples 7 and 8 differ in this case in their glass composition, but have the same IR-reflecting pigment.
  • the curves 71 and 73 are assigned to the embodiment 7 of Table 3, wherein the individual layers differ with respect to the layer thickness.
  • Curve 71 corresponds to the remission curve of the embodiment 7, wherein the coating by 2 printing operations with a sieve of
  • Applied printing has a layer thickness of 11 to 15 ym. The same applies to the
  • Example 8 are assigned from Table 3. The layer thickness of the layer with the curve through 72nd
  • the course of remission shown here is 24 to 28 ⁇ m and the layer thickness of the layer with the remission curve represented by curve 74 is 11 to 15 ⁇ m.
  • the stresses also relax larger deviations of the thermal expansion, without causing flaking or strength problems.
  • Comparative example is.
  • the glass composition also has an influence on the remission in the IR range, whereby this influence increases with increasing
  • Fig. 5 shows the influence of various pigments in the coating on the color location of the coating, determined with a D65 light source measured from the color side in accordance with the measurement standard EN ISO 11664-4.
  • the reference numeral 80 shows the color location of a coating according to the
  • Embodiment 8 from the table.
  • the coating was made by a simple printing process with a screen of mesh size of 77 threads / cm with nominal
  • the color location of the sample 80 is shifted here into the yellow color space.
  • the samples 81 and 82 have a slight yellow shift, in particular sample 81 shows a strong shift in relation to sample 80
  • FIG. 6 shows a schematic representation of the arrangement of the glass panes in one of the prior art
  • the oven door has in this case three thermally toughened glass sheets 8, 9 and 10 with the glass sheet 8 as the outer pane and 10 as the inner
  • disc 10 points into the interior of the oven and disc 8 limits the oven door to the outside.
  • the disks 8 and 9 additionally have coatings 3, 4 on one or two of the surfaces of the glass substrate 1.
  • the outer disk 8 has in this case on the
  • Coating comprising a coating 3 with a transparent, conductive oxide and one on top
  • the decorative layer 4 is an enamel layer containing a black or brown pigment in a glass matrix.
  • the layer 4 acts here as a pure decorative layer, a backscatter from the
  • the central disk 9 has an oxide layer 3 on both sides.
  • FIGS. 7 and 8 show schematic representations of the disc arrangements in the oven according to two
  • the glass substrate 1 without coating has a light transmission Y measured with standard light C / 2 ° of more than 5%, preferably more than 20% and particularly preferably more than 80%.
  • the light transmission Y is measured in the CIE color system. This value applies regardless of the thickness of the substrate, which can usually be between 2 and 10 mm.
  • the substrate material may be transparent, transparent colored by color oxides or have a translucent appearance by light scattering.
  • Light scattering can e.g. in glass ceramic substrates or
  • Crystals are generated in the substrate material.
  • Substrate material of a silicate glass (Si0 2 content> 40 wt .-%).
  • Si0 2 content 40 wt .-%).
  • soda lime glass pane made of a commercially available soda-lime glass used as a substrate. Such soda lime slices are available in various qualities, depending on the iron content.
  • the soda lime glass pane is particularly preferably thermally prestressed. In a further preferred embodiment, it is a floated borosilicate glass, such as the floated glass types BOROFLOAT ® 3.3 or BOROFLOAT ® 4.0 from SCHOTT AG.
  • the layer 2 in this case contains an IR-reflecting pigment with a TSR value of at least 20% and a remission at a
  • the layer 2 acts not only as a decorative layer, but
  • FIG. 8 a development of the invention is shown, in which also in the middle
  • Disk 8 the oxide layers 3 is replaced by the layer 2 according to the invention.
  • a substrate coated according to the invention is outstandingly suitable for use as an outer pane of a multi-pane oven door.
  • a correspondingly coated substrate coated according to the invention is outstandingly suitable for use as an outer pane of a multi-pane oven door.
  • Substrate installed as an outer pane in an oven and the surface temperature on the outside of the
  • the distance of the thermal imager to the outer pane of the oven door was here 203.2 cm.
  • the volume of the oven was 28.317 1 and 5.3 ft 3, respectively.
  • a laboratory measurement setup is described.
  • the respective surface temperatures of the disks were measured with a pyrometer 39 (impac, IE 120 / 82L).
  • the oven door was 50 cm.
  • the volume of the oven was 30x12x12 cm 3 .
  • the distance of the decorated pane to the oven was 2 cm the oven opening has a diameter of 3 cm.
  • the measured slices are
  • FIG. 9 shows a schematic representation of the coverage of the outer pane of the exemplary embodiment with the respective decorative layer.
  • the dimensions of the outer disc are each 29.0 by 20.1 inches. In the outer area of the disc was a with the respective decorative coating
  • the frame 15 leaves a viewing area 16 with the dimensions of 20 by 9.75 inches.
  • this viewing area 16 is the decorative layer applied in the form of a grid pattern 17.
  • comparative measurements were carried out using a glass substrate with an enamel coating 4 with a conventional black pigment as the outer pane.
  • Figures 10 and 11 show schematically the respective construction of the oven door of the embodiment (FIG. 10) and the comparative example (11). In both cases the uncoated side of the substrate points outwards.
  • the middle and the inner pane of the oven door are each coated on one side with a coating 3.
  • the coating 3 contains transparent, conductive oxides.
  • the oven was brought to an operating temperature of 246 ° C or 468 ° C and the temperature determined at various points on the outside of the outer oven disc.
  • Fig. 12 shows the recording of a thermal imaging camera an outer oven door, wherein the oven was heated to 468 ° C with an outer pane according to the invention after a period of operation of 180 minutes.
  • Fig. 14 is a variant of a measuring structure for
  • the oven door has three in this measuring arrangement
  • the coatings 3 are in this case arranged on the facing surfaces of the two inner glass panes.
  • a coating 2 comprising an IR-reflecting pigment, wherein the coating 2 is applied to the side of the glass sheet, which in the
  • the oven door was 203.2 cm. From the thermal images thus obtained, the corresponding temperatures
  • the volume of the oven was 28.317 1 and 5.3 ft 3, respectively.
  • Fig. 15 is a schematic diagram of a measuring arrangement for
  • a laboratory furnace 31 is at a temperature of 450 ° C.
  • the oven has an opening with a diameter of 3 cm. At a distance of 3 cm from this opening, the glass sheet 1 to be measured is placed with the coating 2, wherein the coating 2 in the direction of
  • coated glass pane 1 is equipped with a pyrometer
  • the pyrometer 39 (here is behind the measured to be measured glass substrate 30 and at a distance of 50 cm to be measured
  • FIGS. 16 and 17 show the temperature profile on the outside of different furnace doors as a function of the operating time, with the individual furnace doors differing only by the coating of the outer pane.
  • the surface temperatures were determined by the measurement setup shown in FIG. 14, the oven temperature was 246 ° C. (FIG. 16) and 468 ° C. (FIG. 17).
  • Curve 11 here is to be assigned to the comparative example shown in FIGS. 10 and 12.
  • the curves 12 to 15 and 18 and 19 are different
  • the grid pattern has a diameter of 1 mm (small holes) with a total occupation level of the layer of 64% and 2 mm (big holes) with a total occupancy rate of the layer of 67%.
  • the reference door has a grid pattern with a diameter of 1.5 mm with a total occupancy rate of 63%
  • Table 5 shows the layer compositions of
  • Embodiments according to the curves 12, 13, 14, 15, 18 and 19. The discs have here in the field of view a dot matrix with round, uncoated areas in the
  • Coating is 64% in this design variant.
  • the holes or the uncoated areas within the dot matrix have a diameter of 2 mm.
  • the outside of the disc has a
  • curve 12 corresponds to the temperature profile of the sample 1 from FIG. 5, the applied decorative raster having large holes
  • curve 13 the temperature profile of the sample 10 from table 5
  • curve 14 the temperature profile of the sample 1 from Table 5 with the applied decorraster having small holes
  • curve 19a (only in Fig. 16) of sample 9 from Table 5, with the applied decorraster having large holes
  • Table 5 Embodiments and comparative examples of the temperature measurements shown in FIGS. 16 and 17
  • measuring range 15 represents the surface area with the comparatively highest temperature.
  • the temperature in the measuring range rises sharply up to an operating time of about 60 minutes and then the temperature does not rise or only slightly.
  • the temperature in the measuring range rises sharply up to an operating time of about 60 minutes and then the temperature does not rise or only slightly.
  • Fig. 17 shows the temporal temperature profile at a furnace temperature of 468 ° C, i. the setting pyrolysis of the oven and thus simulates the temperature profile during a pyrolysis process.
  • the measured temperatures increase steeply within the first 60 minutes, and then approach a largely constant value. This value is at all
  • Curve 12 is one here To assign slices with a grid pattern, with which a higher occupancy rate can be achieved than with the
  • Burning process a large part of the heat radiation through the IR-reflecting pigments are reflected in the paste and the heat thus not to melt the glass powder or to form a uniform flow of glass to
  • Pigment content in the coating are adversely affected.
  • the proportion of the pigment in the coating is therefore preferably 10 to 25% by volume, preferably 12 to 20% by volume. -%.
  • Table 6 Determined temperatures of the embodiments shown in Table 5 in baking mode (246 ° F) and pyrolysis mode (875 ° F) Table 6 summarizes and gives the results of the temperature measurements shown in Figs. 16 and 17
  • Samples 1, 3, 4, 9 and 10 correspond to samples 1, 3, 4, 9 and 10 listed in Table 5.
  • the comparative sample is a standard oven door, i. with normal black pigments. From Table 6 shows that the embodiments have a better insulation effect
  • Insulation effect is at least equal to the conventional coatings with transparent conductive oxides.
  • Fig. 18 shows the influence of various
  • compositions in the coating on the color locus of the coating determined with a D65 light source measured from the color side in accordance with the measurement standard EN ISO 11664-4.
  • the samples of area 21 are coatings with a zinc-based glass matrix assigned to the samples of the
  • zinc-based glasses have a shift to yellow color locations while the coatings of the regime 20 are shifted to blue color locations.
  • Fig. 19 shows the in-line transmission profile
  • coated substrates for the Wavelength range between 1.5 ym and 4.5 ym an in-line transmission of at most 0.01%.
  • FIGS. 20 and 21 embodiments are schematically illustrated in which the coating 2 deposited on the glass 1 has pores 32 and 33, respectively. In both cases these are closed pores.
  • Fig. 20 shows an embodiment with largely
  • pores 32 Corresponding pores can be obtained, for example, by the use of calcium carbonate as a blowing agent.
  • the pores 33 shown in FIG. 21 have an elliptical cross section and thus an anisotropic structure. Pores with one
  • pores are present in different sizes and shapes, that is, generally, without being limited to the example shown schematically here, also not round.
  • Fig. 22 and 23 show the temperature profile on the
  • FIGS. 22 and 23 Differentiation of outer pane coating.
  • a laboratory furnace was hereby placed on a
  • FIG. 23 shows a fit obtained by averaging (logistic curve fit with 3 parameters) of the temperature profiles shown in FIG. 22.
  • Samples 13 and 14 correspond to the embodiments shown in FIGS. 16 and 17.
  • the coatings of these embodiments were made without the use of blowing agents.
  • samples 34 to 37 are porous coatings.
  • Coatings therefore have closed pores. All temperature profiles shown in Figs. 22 and 23 were obtained by using the measurement setup shown in Fig. 15. The respective coating compositions were applied to the substrate by screen printing using a 77/55 T screen.
  • Fig. 23 shows that even after a one-hour operating time of the furnace at 450 ° C, the determined on the outside of the disc temperature is below 50 ° C.
  • this maximum temperature can be lowered again. It is assumed that the pores within the coating represent structures on which the IR radiation can be additionally scattered.
  • Blowing agent used When using rice starch as the blowing agent, anisotropic pores having an ellipsoidal cross-section are preferably formed, while the use of CaCO 3 as the blowing agent results in substantially spherical pores.
  • FIG. 23 shows that in the coated glasses 34 and 35, whose pores have a spherical or largely spherical structure, the insulating effect is higher than in the case of the coated glasses 36 and 37 whose coating has ellipsoidal or rice-shaped pores.
  • the blowing agent content in the coating-producing paste 34 is 20% by volume
  • the corresponding paste for preparing the coating 35 contains only 10% by volume of CaCCd as the blowing agent.
  • the sample 35 has a better insulation effect than the sample 34, so that after an operating time of 180 minutes, the maximum temperature of the sample 35 is 0.8 ° C lower than the maximum temperature of the sample 34 among comparable
  • volume-colored substrate is formed, is the
  • Barrier effect of the coating for example, determinable in a test in which a drop of a fluid
  • Medium e.g. Water is applied to the coating and then applied for at least 10 seconds and wiped off after exposure, wherein when looking through the coating through the substrate, the point of contact of the drop is not recognizable as such, if this test is passed.
  • test methods are generally known under the term of visual inspection and are based on the relevant standards, such as DIN EN 1330-10, DIN 25435-2 as well as DIN EN 13018.
  • a direct or indirect visual inspection is favored by an examiner.
  • direct visual inspection the test is carried out with the beam path uninterrupted between the eye of the tester and the surface to be tested, whereas in the case of a test
  • the beam path is interrupted. Furthermore, a
  • the minimum illuminance used in the test is at least 500 ix on the test surface at a distance of less than 600 mm.
  • Viewing angle of the tester is at least 30 °.
  • the examiner preferably complies with the relevant standards, such as DIN EN 13018 and EN 473
  • the exposure time is usually selected as a function of the respective fluid medium considered and can also be more than 10
  • Fluids in the sense of the present disclosure preferably comprise liquids, in particular water, aqueous liquids, alcohols, on these liquids
  • Liquids such as window cleaners, and / or oils and water vapor.
  • the present disclosure comprises the following steps:
  • Liquid in particular a drop, on an area on the surface of the coating of the
  • Standard illuminant D65 or under illumination such as a light bulb, energy saving lamp,
  • Fluorescent lamp or a light emitting diode
  • the illuminance thereby amounts to at least 500 lx at a distance to the coating, ie to the test surface, of less than 600 mm, and c) the viewing angle of the tester is between 5 ° and 90 °, preferably at least 30 °, wherein when the coating is viewed through the substrate, the point of contact of the droplet is not disturbingly visible and, in particular, is not recognizable as such.
  • the above-mentioned visual inspection also referred to as "sidolein test" in the above table, comprises in particular the test as to whether a water edge and / or a water spot is from the coated side
  • window cleaner was used in the test listed in the above table.
  • FIG. 24 shows the influence of the layer thickness of the applied coating on its IR reflectivity.

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Abstract

L'invention concerne un substrat en verre ou en vitrocéramique comprenant une zone de surface présentant un revêtement contenant une matrice de verre et des pigments réfléchissants les IR, les pigments réfléchissant les IR présentant une valeur TSR (réflectance solaire totale), déterminée selon la norme ASTM G 173, d'au moins 20 % et le revêtement présentant, à une longueur d'onde de 1500 nm, une réflectance, mesurée selon la norme ISO 13.468, d'au moins 35 %. En outre, l'invention concerne une pâte pour la fabrication d'une couche réfléchissant les IR, en particulier sur un substrat en verre ou en vitrocéramique, comprenant au moins un pigment réfléchissant les IR et une poudre de verre ainsi qu'un procédé pour la fabrication d'un substrat revêtu correspondant.
EP18811184.3A 2017-11-22 2018-11-22 Revêtement décoratif doté d'une réflexion augmentée des ir Pending EP3713888A1 (fr)

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DE102017127624.6A DE102017127624A1 (de) 2017-11-22 2017-11-22 Beschichtetes Glas- oder Glaskeramik-Substrat, Beschichtung umfassend geschlossene Poren sowie Verfahren zur Beschichtung eines Substrats
US201862712615P 2018-07-31 2018-07-31
PCT/EP2018/082247 WO2019101873A1 (fr) 2017-11-22 2018-11-22 Revêtement décoratif doté d'une réflexion augmentée des ir

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EP18811184.3A Pending EP3713888A1 (fr) 2017-11-22 2018-11-22 Revêtement décoratif doté d'une réflexion augmentée des ir

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CN (2) CN111587231B (fr)
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DE (1) DE102017127624A1 (fr)
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WO (3) WO2019101878A1 (fr)

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CN111670171A (zh) 2020-09-15
WO2019101878A1 (fr) 2019-05-31
US20200354264A1 (en) 2020-11-12
US11673826B2 (en) 2023-06-13
US11420901B2 (en) 2022-08-23
BR112020010342A2 (pt) 2020-11-10
EP3713889A1 (fr) 2020-09-30
CN111587231B (zh) 2023-01-13
WO2019101873A1 (fr) 2019-05-31
BR112020010277A2 (pt) 2020-10-13
US20200283333A1 (en) 2020-09-10
MX2020005171A (es) 2020-08-20
US20230035460A1 (en) 2023-02-02
CN111587231A (zh) 2020-08-25
WO2019101880A1 (fr) 2019-05-31
DE102017127624A1 (de) 2019-05-23
MX2020005248A (es) 2020-08-24

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