WO2012059088A2 - Composition de couleurs vitrifiables en céramiques pour la fabrication de décors cuits, procédé pour leur fabrication et procédé de fabrication d'un revêtement décoratif - Google Patents

Composition de couleurs vitrifiables en céramiques pour la fabrication de décors cuits, procédé pour leur fabrication et procédé de fabrication d'un revêtement décoratif Download PDF

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Publication number
WO2012059088A2
WO2012059088A2 PCT/DE2011/001942 DE2011001942W WO2012059088A2 WO 2012059088 A2 WO2012059088 A2 WO 2012059088A2 DE 2011001942 W DE2011001942 W DE 2011001942W WO 2012059088 A2 WO2012059088 A2 WO 2012059088A2
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ceramic
diffusion
glass
noble metal
inhibiting
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PCT/DE2011/001942
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German (de)
English (en)
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WO2012059088A3 (fr
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Khwan-Khung Lim
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Khwan-Khung Lim
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0551—Flake form nanoparticles
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
    • C03C17/04—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass by fritting glass powder
    • 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
    • C03C3/076—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
    • C03C3/089—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
    • 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
    • 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
    • C03C8/18—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing free metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0009—Pigments for ceramics
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0078—Pigments consisting of flaky, non-metallic substrates, characterised by a surface-region containing free metal
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • C03C2217/479—Metals
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/72—Decorative coatings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/80—Optical properties, e.g. transparency or reflexibility
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1004—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2
    • C09C2200/1008—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2 comprising at least one metal layer adjacent to the core material, e.g. core-M or M-core-M
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
    • C09C2200/1025—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin comprising at least one metal layer adjacent to core material, e.g. core-M or M-core-M

Definitions

  • the invention relates to a ceramic melt color composition, a process for their preparation and a process for producing a decorative coating on glass, enamel or Keramikober surfaces with the ceramic melt color composition.
  • at least one noble metal is directly present in the ceramic melt color composition or platelets coated with precious metal are contained in the ceramic melt color composition.
  • enamel composition can also be used in a glaze, a glass or a ceramic to color it.
  • Ceramic decorative paints as well as chandelier and precious metal Preparations are known to be very often used for the decoration of ceramic and silicate surfaces. These objects to be decorated include porcelain, bone china, vitreous china, stoneware, stoneware, enamel, tile and glass.
  • Decorative paints are enamel paints or glass paints, onglaze paints or inglaze paints, which usually consist of frits or glass flow and color bodies necessary for dyeing.
  • the decorative colors are also characterized by a melting phase that arises during the fire, which encloses the color bodies contained therein and can be baked to a homogeneous decorative layer.
  • colloidal gold has been known in principle for a long time as Cassius 1 gold gold purple (eg, Gmelin, Handbook of inorganic chemistry, Bd. Au, 399-400, 1954). These effects of gold and / or silver have been used since ancient times to dye glass and thereby color impressions in pink, red, yellow, blue, ruby red, violet, among others achieved.
  • the ceramic magenta colors are color bodies which contain gold and silver or only gold in colloidal form. With the silver content of purple colors, the red color of the color can be influenced by red violet, purple, red and reddish brown. Depending on the diffusion of the gold and predominantly of the silver in the decorated ceramic surface, the shades are very different.
  • the previous precious metal decorations are made from precious metal embossments, such as bright gold / platinum, matte gold / platinum, polished gold / platinum. These consist of solutions of organic gold, platinum and palladium compounds. As flux, certain organic metal compounds are usually used to influence the adhesive strength and optical properties of the metal film on the substrate.
  • the main component is gold.
  • precious metal preparations are usually made of gold and smaller additions of platinum and / or palladium. During the firing, these precious metal preparations lack a melting phase, since a normal melting phase can not tolerate the noble metal preparations in a common application.
  • Polished gold also referred to as matte gold, contains very high gold content in the range 15% by mass to 60% by mass. It consists partly of gold powder. Subsequent polishing is necessary to give a fine appearance. In powder gold, high-grade gold powder is also used to achieve a massive gold appearance. These are called all counted among the precious metal preparations.
  • a chandelier preparation has a lower proportion of gold and often additionally contains a proportion of dissolved metal compounds, such as Zr, Fe, Co, Ti, Cr, Mn and Zn. It has an iridescent luster gloss and various colors can be obtained depending on the metal composition.
  • EP 1 559 692 B1 and DE 10 122 762 A1 describe how a precious metal preparation and chandelier can be prepared from solutions orga- nischer gold, palladium and platinum compounds can be put together. As a flux, certain organic metal compounds are usually used.
  • DE 102 57 087 B4 discloses a process for producing a precious metal decoration on glass, ceramic or metal.
  • the noble metal flakes may be mixed with conventional bright noble metal preparations, with soluble organic metal compounds contained in liquids, with finely powdered glass flux such as lead borosilicate or alkali borosilicate, or silver powder.
  • the resulting mixture in which coated flakes are to be contained in a proportion of 20% by mass to 80% by mass, may be mixed with an oil and screen printing with a screen printing standard medium.
  • the decorative preparation should then contain 4% by mass to 50% by mass of coated platelets.
  • Silver is elemental and / or ionic and gold predominantly elementary. It can be brilliant reddish and / or warm shades, especially for purple color for
  • Multi-color decor layers find a meaning to be obtained.
  • the color used should contain a coloring component in addition to a glass flow.
  • the coloring component is intended to include at least one metal selected from the group consisting of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Au, Ru, Rh, Pd Os, Ir, Pt, and / or a compound of the metal loaded molecular sieve included.
  • the molecular sieve should be an aluminosilicate-based zeolite or a silicate.
  • a further object is a decoration of an impression of a specular, shiny precious metal forth, a high scratch resistance, dishwasher resistance and good adhesion of the decorative coating is maintained, the cost by reducing the proportion of particularly expensive precious metals, especially gold, to be reduced.
  • this object is achieved with a ceramic melt color composition according to claim 1.
  • a process for their preparation is specified in each of claims 11 or 17. With the ceramic melt color composition can a
  • the inventive ceramic melt color composition can be used for the production of decors on glass, enamel or ceramic surfaces. You can also call them color.
  • the maximum 50% by weight should be selected if the diffusion-inhibiting flux component (s) is / are directly incorporated in the noble metal platelets / particles or the noble metal-coated platelets / particles. Otherwise, the maximum share may be ten times that.
  • the minimum proportion of diffusion-inhibiting flux component (s) should be 1% by mass, preferably 2% by mass.
  • the diffusion-inhibiting flow component (s) may be incorporated directly or indirectly into the noble metal platelets / particles and / or as platelets coated with noble metal.
  • the diffusion-inhibiting flow component (s) and / or glass flow can be incorporated directly or directly into the noble metal (s) by CVD, PVD, a milling process, a gas phase process, a precipitation process, laser ablation and / or electrochemical processes.
  • the character of a ceramic enamel color can be achieved by at least one diffusion-inhibiting flow component.
  • the noble metal (s) may be selected from Au, Pt, Ag, Pd, Ru, Ir and Os. It is also possible to use an alloy of at least one of these noble metals.
  • the diffusion-inhibiting flux component may be selected from Cr, Mn, Fe, Co, Ni, Cu, Zn, Si, V, Sn, Ti, Al, Bi, In, W, Ta, Zr, Y, Nb, Ce, Mo, Cd , Sb, Ge, In, Li, Na, Mg, K, Ca and Sr.
  • Cr, Mn, Fe, Co, Ni, Cu, Zn, Si, V, Ba, B, PB and Sn are preferable.
  • a salt, a hydrate, a sol, an oxide, a glass, a carbide or a nitride of these chemical elements can also be used as the diffusion-inhibiting flux component. It can also be colloidal be used.
  • an oxide layer protecting the surface of the precious metal (s) can be achieved during the baking of the decorative coating which diffuses precious metal into a glaze or the material on which the
  • Precious metal can also be used with a medium
  • Particle size may be included in the range 1 nm to 500 nm.
  • the proportion of precious metal contained should be in the range of 1% by mass to 35% by mass.
  • the noble metal particles can be obtained by the following manufacturing processes: grinding processes, in particular high energy milling in ball mills, ultrasonic reactors, reactive grinding, gas phase processes, flame reactor processes, plasma reactors, laser reactors, hot wall reactors, precipitation processes, sol-gel processes or hydrothermal synthesis.
  • An additionally contained glass flux can be treated with at least one metal oxide, a mixed oxide, a silicate, a glass with Si, Li, Na, Zn, Zr, B, K Mg, Ca, Al, Bi, Cd, Pb, La, Ti, Sn, Ce, Fe, V, Nb, Ta, Mn, Co, Cu, Ni, In, Ge, and / or P is formed.
  • a diffusion-inhibiting flow component can also included at least one organic and / or inorganic chemical compound of base metals, which are contained in the groups Ia, Ib, 2a, 2b, 3a, 3b, 4a, 4b, 5a, 5b, 6b, 7b and 8b of the Periodic Table be.
  • It may be an organic and / or inorganic compound which is at least one metal selected from, Ru, Al, V, Sn, Bi, Ni, Cr, Co, Os, Ir, Fe, Zr, Ta , Si, B, Mn, W, Ce, Mo, Ba, Pb, Ge, Ca, Ti, Cu, Zn, Ga, Li, Na, K, Be, Mg, Cd, Sr, Sr, In, Nb and Rh , is formed.
  • These organic and / or inorganic compounds may convert to glass or oxides during or after the firing.
  • organic or inorganic compounds examples include carboxylic acids, such as ethylhexanoates or octanoates, pentanedionates, resinates,
  • the at least one diffusion-inhibiting flow component can be present in a size range between 1 nm and 1 .mu.m. It may be present in the nanoscale range between 1 nm and 100 nm or in the submicrometer range between 100 nm to 1 ⁇ .
  • the employed in the ceramic melting colors composition glass flow / can may preferably Si0 2, Sn0 2, ZnO and / or B 2 0 3, the / which should form the main component in the glass flow (s), and also Li0 2, Na 2 0, Zr0 2 , B 2 0 3 , K 2 0, MgO, CaO, Al 2 0 3 and / or Bi 2 0 3 be contained.
  • the last-mentioned oxides should be contained in a smaller proportion than the Si0 2 , Sn0 2 , ZnO or ⁇ 2 0 3 .
  • Precious metal and diffusion-inhibiting flux component (s) should have a content of ⁇ 25% by mass, preferably ⁇ 20 Mass% may be included in the ceramic melt composition, so that the glass flow rate is significantly higher, in the event that a Glas raw material is present.
  • the ceramic melt color composition can be dispersed in organic components so that it then has a consistency suitable for printing, preferably screen printing.
  • organic components are used for the production of screen-printing inks or dyes. and are commercially available.
  • the organic components can account for a proportion in the range of 35% by mass to 65% by mass in relation to the previously described color composition.
  • Polyamide resin, rosin resin, asphalt resin, phenol resin, ketone resin, epoxy resin, acrylic resin, polyurethane and / or maleinate resin may be contained as binders.
  • a suitable for example for application to a surface consistency can be achieved with a suitable solvent.
  • oils preferably essential oils, bitumen and a modified phenolic resin as available under the trade name Dymerex.
  • a ceramic melt color composition according to the invention with precious metal and / the diffusion-inhibiting flux component (s) can be used with a sol-gel, CVD or PVD process, electroless deposition, electroplating or a combination thereof.
  • the ceramic enamel composition is applied as a layer on a temporary support, then the
  • noble metal and diffusion-inhibiting flux component (s) can be applied simultaneously and together in one layer at least in CVD or PVD processes. It may also be formed, a multilayer structure may be gebil ⁇ det in which individual layers of precious metal or diffusionshemraender flow component. Precious metal and other metals can but also deposited as an alloy in layer form.
  • At least one layer of Si0 2 can be formed before the
  • Layer structure is removed from the carrier.
  • a carrier thin flexible polymer films can be used. During the coating, such a film can be unwound from a roll, coated and rolled up again, which is particularly effective in vacuum coating.
  • the film may have been previously coated with a release layer on which the layer structure for the ceramic melt color composition is applied. This release layer can be dissolved, but at least dissolved, for the detachment of the layer structure, for example with a solvent.
  • the coating may be on a polymeric film, such as a peelable acrylate film formed on a PET film.
  • This film can be removed from the film after coating, then dissolved as already mentioned or else applied directly with the coating on a surface to be decorated with a decor and then baked at appropriate temperatures, the decor.
  • the film After removal of the film with coating from the film, the film can be re-coated with acrylate and reused for PVD or CVD coating.
  • the film may also contain components of the glass flux. These components of the flow can also be applied as a layer, with a
  • Multi-layer structure can be formed.
  • glass flow components may also be used in the polymeric film material, such as e.g. the acrylate, contained or embedded therein.
  • the film can thus be applied directly to the surface to be decorated with the décor after the removal of the film, and the decoration can be baked during the heat treatment, without additional work steps being required, since all the necessary components for the decoration are contained in the film can.
  • the proportion of diffusion-inhibiting flux component should be kept as high as possible with respect to the proportion of precious metal at a maximum of 30% by mass in order to be able to optimally exploit the desired effect. This is especially true when manufactured with a vacuum coating process.
  • the ceramic melt color composition can be prepared such that metal oxide, mica or glass flakes by electroless deposition, galvanic, with a CVD or PVD method or hydrolysis reaction / reduction with
  • Precious metal and the diffusion-inhibiting flow component (s) are coated and the coated platelets for the ceramic melt color composition are then mixed with the glass flux.
  • the ceramic melt composition which has a consistency suitable for printing by means of organic components, is applied to a glass, enamel,
  • Ceramic surfaces or a surface of a temporary support member applied Subsequently, it is subjected to a heat treatment in which the organic components are expelled and the decorative coating is baked.
  • the decorative coatings produced on the glass, enamel and various ceramics according to the invention had a high metallic brilliance, did not change their visually perceptible impression and remained securely on the surface even after more than 1000 rinses in a dishwasher without
  • all constituents contained in the ceramic melt composition can be made very small and mean particle sizes in the nanometer range, that is at least smaller than 1 micrometer, can be maintained. For the glass flow but also larger particle sizes can be left to.
  • the precious metal content can be very small and thus the Costs are kept low.
  • the respective coloration can be influenced by the precious metal used, the diffusion-inhibiting flux component (s) and / or the composition of the glass flux.
  • a resistant decorative coating can be achieved by covering the precious metal flakes / particles or the platelets coated with precious metal with a glass flow.
  • the decorative laminations producible with the invention have an optically metallic gloss, as would be the case with a pure metal layer.
  • a suitable selection of the diffusion-inhibiting flow component (s) and / or the components contained in the glass flow a certain coloration can be achieved, which differs from the actual ceramic melt color composition of the noble metal used.
  • gold-shining decorative coatings can be obtained with silver.
  • Decorative coatings can be used as a reflector. They are also microwaves suitable.
  • the decals produced according to the invention or to be produced with the ceramic composition of the invention to tarnish with silver platelets / particles or silver-containing platelets / particles through an oxide and / or glass layer, that worsens the visual impression to avoid.
  • the invention will be described below by way of example. Showing:
  • FIG. 1 shows in schematic form an example of a decorative coating produced according to the invention
  • FIG. 2 shows in schematic form another example of a decorative coating produced according to the invention
  • FIG. 3 shows an example of a decorative coating formed on a substrate surface
  • FIG. 4 shows a further example of a decorative coating formed on a substrate surface
  • FIG. 5 shows a further example of a decorative coating formed on a substrate surface
  • FIG. 6 shows a further example of a decorative coating formed on a substrate surface.
  • a decorative coating is formed on the surface of a substrate 5.
  • the substrate 5 may consist of a porcelain, Bone / Vitreous China, stoneware, tile, glass or enamel.
  • the stoving temperatures are between 480 ° C.-650 ° C., for glass and enamel, or in the range 780 ° C.-900 ° C. for onglaze firing for porcelain, bone / vitreous china, stoneware / ware and for tiles or between 1150 ° C - 1250 ° C at Inglaze brand for porcelain.
  • FIGS. 1 and 2 show examples of decorative coatings produced according to the invention.
  • precious metals 2 with an average particle size are precious metals 2 with an average particle size
  • the noble metals 2 are deposited almost in a layer form either first on a surface of a temporary support element or directly on a substrate 5 made of porcelain, bone / vitreous china, stoneware / good, tile, glass or enamel, and later of a diffusion-inhibiting flow component 1 as a second cover layer enclosed and covered.
  • a middle plate 6 made of polymer, metal oxide, ceramic, mica or glass is formed and indirectly surrounded by noble metal 2.
  • the whole is of another diffusion-inhibiting
  • the diffusion-inhibiting components 1 and 4 may be formed in the form of a metal and a salt, a carbide, nitride, oxide, glass or an alloy of the metal. These platelets coated with noble metal and additionally having at least one diffusion-inhibiting flux component 1 and / or 4 can be treated by a process such as solgel, CVD, PVD, electroless plating or electroplating or a combination of this method.
  • the diffusion-inhibiting flux component 1 and the noble metal 2 are constructed in a common layer and surrounded by further diffusion-inhibiting flux component 4.
  • the platelets coated with noble metal and the diffusion-inhibiting flow components are obtained in a glass flux, which leads to the improvement of adhesive strength and machine rinse resistance.
  • the noble metal 2 is formed as an inner plate, whereupon the diffusion-inhibiting flow components 1 and 4 are formed.
  • the noble metal 2 and the diffusion-inhibiting flux component 1 are in a layer which is enclosed by the second diffusion-inhibiting component 4.
  • Carrier made with a release layer
  • Methyl methacrylate resin first provided with a SiO x layer by reactive sputtering.
  • this SiO x layer reached a thickness of 10 nm.
  • Chromium and titanium are diffusion-inhibiting components
  • the coated PET film was treated with acetone, thereby slowly dissolving the methyl methacrylate resin with the acetone.
  • the coating with the metal layer can thus be separated from the temporary support and then stirred in an intensive stirrer at high speed for one hour.
  • the coating of metal and SiO x was crushed into platelets / particles.
  • the metal flakes / particles dispersed in the acetone could be separated from the resin content in a filter press.
  • the resulting filter cake was then dried at 80 ° C for 0.5 hours.
  • the resulting metal flakes / particles had a high brilliance and had an average particle size of about 25 ⁇ on.
  • the proportion of silver was 70% by mass, that of chromium 20% by mass and that of titanium 10% by mass.
  • a frit was made with the following composition: Settlement 48.5 mass% S1O 2 , 9.2 mass% Li0 2 , 3.2 mass% Na 2 O, 1.8 mass% ZnO, 5.8 mass% 2r 2 0 and 31 , 5 mass% B 2 0 3 used.
  • the glass frit had an average particle size of 15 ⁇ .
  • the metal-glass frit obtained after mixing was mixed with the following organic components to give a screen-printing consistency:
  • Degalan 540L commercially available from Evonik Industries
  • DOP dioctyl phthalate
  • Shelsol AB commercially available from Shell
  • 0 r 01 by mass BYK 066 commercially available from BYK Chemie
  • 18.2 mass% of polyol commercially available from Celanese.
  • the metal content in the paste suitable for printing was 5% by mass, the glass content was 45% by mass, and the content of organic components was 55% by mass.
  • the decorative coating was baked and formed with the flow of a protective glaze.
  • temperatures were 780 ° C to 850 ° C and selected for a rapid fire 860 ° C to 900 ° C.
  • the metal flakes / particles were prepared as in Example 1.
  • the glass flow had the following composition:
  • a mixture was prepared by stirring at a temperature of 120 ° C., in which the solids were distributed homogeneously, the metal platelets / particles had a proportion of 8% by mass, the flux a proportion of 52% by mass.
  • the printable paste was applied to a glass surface with an edger and then subjected to a heat treatment at temperatures in the range of 480 ° C to 650 ° C for baking.
  • the ceramic platelets were coated as uniformly brightly after the reduction of the AgNO 3 with silver. Alternatively, however, such platelets can also be galvanically coated with silver.
  • the filter cake was placed in a liquid which was dissolved with 0.5 g of SnCl 2 in 100 ml of deionized water, 4 g of NaOH dissolved in 250 ml of deionized water and 1 g of Na 2 CsH 5 O 7 in Dissolved 450 ml of deionized water was formed. This mixture was stirred at 70 ° C for 0.5 hours, then washed with water and filtered. The metal content then had the following composition 80 mass silver, 8 mass% platinum, as precious metals and
  • the so coated platelets can be used in this form for a ceramic melt color composition for
  • Decorative coatings are used. But they can also be provided with a protective layer, for example Si0 2 .
  • a protective layer for example Si0 2 . This can be achieved in a liquid formed with 1000 ml of isopropanol, 9 g of a 28% aqueous NH 4 OH solution and 140 g of tetraethoysilane, into which the metal-coated platelets can be added. The solution containing the platelets was stirred for 10 hours at room temperature, then washed in water, filtered and in a circulating air dryer at 85
  • the coated plates were annealed at 850 ° C for 0.5 hours.
  • the flux used in this example had the following composition: 68 mass% Si0 2 , 2.8 mass% Li 2 0, 2 mass% Na 2 0, 6.2 mass-5 A1 2 0 3 , 4, 8 mass -%
  • the decorative coating was baked at temperatures in the range of 1150 ° C to 1250 ° C. She was shiny.
  • coated platelets according to Example 3 are used with a flow of the composition according to Example 1.
  • a metal content ie silver with diffusion-inhibiting flow components platinum and tin of 5 mass%, a glass content of 55% by mass and organic components for producing a printable paste with a share of 40% by mass has been selected.
  • the organic components of Examples 1 or 3 can be used, it being possible for the proportions of the individual oxides to be modified proportionally.
  • the decorative coating is particularly suitable for porcelain, bone china, vitreous china, stoneware and stoneware.
  • Example 3 With metal coated platelets according to Example 3 a glass flow according to Example 2 (metal content 6% by mass, glass content 50% by mass) and 44% by mass of a marginal medium according to Example 2 was in the multiply described form by means of a roll mixer a printable paste produced with homogeneous distribution of solids and with a conventional
  • the decorative coatings as prepared in Examples 1 to 5 described may also be provided with at least one protective layer as mentioned in the general part of the description.
  • the protective layer (s) can be formed on the surface to be provided with the decorative coating and / or also on the surface of the decorative coating.
  • Example 1 There were metal flakes / particles of Example 1 with a share of 10% by mass, 2.5% by mass in
  • a diffusion-inhibiting flow component is produced as follows:
  • This mixture is heated to 90 ° C and held the temperature over a period of 30 min, with simultaneous stirring.
  • the total mass is reduced to 450 g.
  • This dispersion is then mixed with the diffusion-inhibiting flow component and homogenized in a roll mixer.
  • the total mass of the mixture is reduced to 500 g.
  • a printable paste can be obtained, which is used for the production of decors and thereby by means of a polyester mesh 120-140 threads / cm either directly on the surface of a glass or ceramic product or indirectly by means of a decal on porcelain, bone China, Vitreous China . Stoneware or stoneware can be applied.
  • the decor can be baked. This gives a platinum-white decoration that has a visual impression of a decoration made of pure platinum precious metal preparation.
  • diffusion inhibiting flux component 17.51 mass% diffusion inhibiting flux component, 72.49 mass% organic constituents.
  • the proportion of diffusion-inhibiting flux component is above 50% by mass based on the noble metal.

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Abstract

L'invention concerne une composition de couleurs vitrifiables en céramiques, un procédé pour leur fabrication et un procédé de fabrication d'un revêtement décoratif sur des surfaces de verre, d'émail ou de céramique avec la composition de couleurs vitrifiables en céramiques. L'invention vise à mettre au point des possibilités de fabrication de décors contenant des métaux nobles sur des surfaces de verre, d'émail ou de céramique, qui conservent durablement l'effet optique d'un métal brillant pur, qui offrent une résistance élevée aux rayures et une bonne adhérence du revêtement décoré. La composition de couleurs vitrifiables en céramiques selon la présente invention contient, en dehors de plaquettes/particules de métaux nobles et/ou de plaquettes revêtues de métaux nobles, en plus au moins un composant de flux empêchant la diffusion, avec une proportion maximale de 50 % en masse par rapport au métal noble contenu. Si le ou les composants de flux empêchant la diffusion sont directement intégrés dans le métal noble, le ou les composants de flux empêchant la diffusion peuvent représenter une proportion plus élevée que lorsqu'ils se trouvent dans une matrice conjointement avec les plaquettes/particules de métal noble et/ou avec les plaquettes/particules revêtues de métal noble.
PCT/DE2011/001942 2010-11-02 2011-11-02 Composition de couleurs vitrifiables en céramiques pour la fabrication de décors cuits, procédé pour leur fabrication et procédé de fabrication d'un revêtement décoratif WO2012059088A2 (fr)

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WO2016154822A1 (fr) * 2015-03-27 2016-10-06 华为技术有限公司 Plaque en verre coloré utilisée pour des bornes, son procédé de formation et borne
WO2018163133A1 (fr) 2017-03-10 2018-09-13 Merck Patent Gmbh Préparation métallique et revêtements fabriqués à partir de celle-ci
CN112499969A (zh) * 2020-11-12 2021-03-16 广东健诚高科玻璃制品股份有限公司 一种玻璃浆组合物及其制备方法与应用

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CN111765716A (zh) * 2020-07-09 2020-10-13 长虹美菱股份有限公司 一种光催化抗菌自洁净触控板

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WO2016154822A1 (fr) * 2015-03-27 2016-10-06 华为技术有限公司 Plaque en verre coloré utilisée pour des bornes, son procédé de formation et borne
WO2018163133A1 (fr) 2017-03-10 2018-09-13 Merck Patent Gmbh Préparation métallique et revêtements fabriqués à partir de celle-ci
CN110337470A (zh) * 2017-03-10 2019-10-15 默克专利股份有限公司 包含金属颗粒的涂料组合物
CN110382632A (zh) * 2017-03-10 2019-10-25 默克专利股份有限公司 金属制剂及由其制备的涂层
JP2020510733A (ja) * 2017-03-10 2020-04-09 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ 金属粒子を含有するコーティング組成物
JP2020522608A (ja) * 2017-03-10 2020-07-30 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ 金属配合物およびそれから作製されたコーティング
CN114181559A (zh) * 2017-03-10 2022-03-15 默克专利股份有限公司 金属制剂及由其制备的涂层
CN110337470B (zh) * 2017-03-10 2022-04-05 默克专利股份有限公司 包含金属颗粒的涂料组合物
CN112499969A (zh) * 2020-11-12 2021-03-16 广东健诚高科玻璃制品股份有限公司 一种玻璃浆组合物及其制备方法与应用

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