US20030075079A1 - Glazing pigment and method for the production thereof - Google Patents

Glazing pigment and method for the production thereof Download PDF

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Publication number
US20030075079A1
US20030075079A1 US10/203,012 US20301202A US2003075079A1 US 20030075079 A1 US20030075079 A1 US 20030075079A1 US 20301202 A US20301202 A US 20301202A US 2003075079 A1 US2003075079 A1 US 2003075079A1
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Prior art keywords
oxide layer
layer
metal
backing
substrate
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US10/203,012
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Inventor
Gunter Sommer
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Eckart GmbH
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Eckart GmbH
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Application filed by Eckart GmbH filed Critical Eckart GmbH
Assigned to ECKART GMBH & CO. KG reassignment ECKART GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SOMMER, GUNTER
Publication of US20030075079A1 publication Critical patent/US20030075079A1/en
Priority to US10/900,226 priority Critical patent/US7217318B2/en
Assigned to ECKART GMBH reassignment ECKART GMBH CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: ECKART GMBH & CO. KG
Abandoned legal-status Critical Current

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    • 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
    • C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02—Preparations containing skin colorants, e.g. pigments
    • 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
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0018—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings uncoated and unlayered plate-like particles
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • C09C1/0051—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index
    • 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
    • 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
    • C09C1/36—Compounds of titanium
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    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/36—Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005—Separation of the coating from the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/085—Oxides of iron group metals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
    • 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
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    • 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
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1037—Interference pigments characterized by the core material the core consisting of an inorganic suboxide or a mixture thereof, e.g. SiOx or TiOx
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1054—Interference pigments characterized by the core material the core consisting of a metal
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1087—Interference pigments characterized by the core material the core consisting of bismuth oxychloride, magnesium fluoride, nitrides, carbides, borides, lead carbonate, barium or calcium sulfate, zinc sulphide, molybdenum disulphide or graphite
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/24—Interference pigments comprising a metallic reflector or absorber layer, which is not adjacent to the core
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/301—Thickness of the core
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/302—Thickness of a layer with high refractive material
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    • C09C2220/00—Methods of preparing the interference pigments
    • C09C2220/10—Wet methods, e.g. co-precipitation
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    • C09C2220/00—Methods of preparing the interference pigments
    • C09C2220/10—Wet methods, e.g. co-precipitation
    • C09C2220/103—Wet methods, e.g. co-precipitation comprising a drying or calcination step after applying each layer
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    • C09C2220/00—Methods of preparing the interference pigments
    • C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed

Definitions

  • the invention relates to a nacreous pigment and a method for the manufacture thereof, in which a multilayer film is produced by vacuum evaporation coating on a substrate and, after release from the substrate, the particles thus produced are comminuted into pigment particles of the desired size, vapor deposition of a plurality of layers taking place at separate locations within an evacuable container and the substrate being passed along the sources of evaporation.
  • interference phenomena may occur in pigments of the generic type.
  • Nacreous pigments are used in lots of fields of application, in particular for decorative purposes, car paints, cosmetic purposes or in the field of safety printing.
  • an inorganic salt for example sodium chloride
  • an inorganic salt for example sodium chloride
  • German patent application 199 02 141 which is no prior publication. It specifies, by vapor deposition, to produce a reflecting or substrate layer of aluminum, on which, by subsequent evaporation, to deposit a transparent layer, for instance of magnesium fluoride or titanium oxide.
  • DE 12 42 778 provides that the vapor-deposited layers consist of the group of zinc sulfide, zinc oxide, guanine, magnesium fluoride, titanium dioxide, calcium fluoride and cryolite, with a material from the group of alkali halides, alkaline earth halides or alkali borates, such as Na 2 B 4 O 7 ; B 2 O 3 ; MgCl 2 , being used as a substrate for these films.
  • Evaporation temperatures depend on the respective chromogenic substance or substrate.
  • Interference phenomena are employed for chromogenic purposes by exploitation of the path difference of the light waves that is determined by reflection on the interfaces produced by the various deposited layers. These effects of interference are affected by the thickness of the individual layers and the index of refraction thereof. In the case of an uncolored pearlescent pigment, the product of film thickness in nm and refractive index is to remain within a range between 10 and 200.
  • Interference colors are produced when this product is in a range above 200, the brightest colors occurring with a given pigment weight concentration in the range of 200 to approximately 1500. Color intensity also depends on the uniformity of platelet thickness i.e., on the plane parallelism of the substrate and the plane parallelism of the deposited layers, because pigment platelets of irregular thickness reflect varying colors which may cancel one another so that there is no color effect or no production of pure colors.
  • Liquid-phase or gas-phase precipitation leads to significant porosity, frequently of more than 25 percent of the layer. This porosity lessens the intensity of the reflected light.
  • vacuum evaporation coating also using electron beams—sputtering and the CVD method are specified as methods known per se.
  • these methods are mentioned to be rather costly and therefore used only for optical lenses, filters and the like.
  • TiO 2 flakes As for the production of TiO 2 flakes, continuous film fragmentation is mentioned as a familiar method, the films being produced for instance by thermal hydrolysis of TiOCl 2 .
  • Alternatives consist in the deposition of titanium alkoxide on a surface and fragmentation of the resulting film by vapor treatment, in depositing colloidal TiO 2 solution on a glass surface and scratching off the resulting film.
  • Mention is also made of the application of a TiOCl 2 solution on a gelatin film and detachment of the gelatin film, vacuum deposition, acid treatment of potassium titanate and subsequent heating, or the production and fragmentation of hollow TiO 2 particles from a mix of a surfactant with a colloidal TiO 2 solution.
  • Substrate-free TiO 2 flakes may also be obtained by the substrates being dissolved in strong acids or bases.
  • TiO 2 coated mica from a TiOCl 2 solution
  • the TiO 2 layers obtained may be coated with organic dyes as well as with thin layers of silver, nickel or compositions of various metals in order to obtain a darker shade.
  • DE-AS 1 136 042 teaches to use substrates of a low refraction index in the form of oxides or oxide hydrates of metals of the IVth and/or Vth group, for example SiO 2 , and to coat them with substances of a higher refraction index, for example oxides of Ti, Fe, Sb, Sn etc.
  • the production of the platelets there described is implemented by a glass, ceramic, metal or plastic substrate being wetted with a solution of a hydrolysable compound of the metal that is to be converted into the desired oxide; from the liquid film thus produced, the respective oxide or oxide hydrate is formed as a thin coating by subsequent heating.
  • U.S. Pat. No. 3,438,796 teaches to produce pigment platelets that consist of a plurality of films of silicon oxide and aluminum, with the silicon film serving as a protective layer for the aluminum on the one hand and for producing interference effects in dependence on its thickness on the other.
  • the aluminum film may be adjusted in thickness so that it is substantially impermeable to light.
  • the layers are produced by chargewise vapor deposition.
  • EP 0 803 549 provides silicon oxide layers to be vapor-deposited on conventional platelet particles of a length of for instance 1 to 200 ⁇ m.
  • the platelets must consist of a metallically reflecting material or metal alloys. Alternatively, the use of mica may be considered. It further specifies that it is a familiar way of proceeding to deposit, on such a substrate of a colorless oxide, crystallized titanium oxide layers, for instance in the form of rutile, on which to deposit another layer of colored inorganic material such as iron oxide.
  • this object is attained by at least one backing layer, in particular a silicon oxide backing layer, and at least one metal oxide layer, in particular a titanium oxide layer being vapor-deposited on the substrate, in particular a circulating metal belt.
  • the silicon oxide layer thus deposited helps create a backing which, after being peeled off the substrate, namely the metal belt, excels by high plane parallelism and defined thickness in particular as compared to natural mica platelets, but also to platelets produced by wet-processing.
  • the SiO starting material used according to the invention does not have any impurities, for instance iron. Further, there is no need of complicated preparation such as calcination, comminution, grading etc.
  • the backing according to the invention also has advantages over synthetic mica (phlogopite), which has never gained any commercial importance because of complicated manufacturing requirements at high pressure and elevated temperature.
  • the vapor deposition rate and oxygen partial pressure help regulate the optical properties such as the refraction index and reflection coefficient of the backing, it being possible in this way to produce defined and reproducible shades and changes of color in dependence on the angle of view.
  • the thickness of the layer that is vapor-deposited subsequently in particular a titanium oxide layer, can also be regulated as desired through the vapor deposition rate and/or the metal belt velocity, possessing excellent plane parallelism due to the plane surface of the previously deposited silicon oxide layer.
  • the pigments produced according to the invention are plane parallel as far as to the outer edge. The result is higher color purity and improved luster even in minor particles, because the scattered-edge portion is minimized.
  • the pigment platelets peeled off the backing have largely identical and reproducible optical properties, for example the same shade of color when viewed from a certain angle.
  • the pigments obtained according to the invention have great shear stability. This is due to the fact that excellent bonding of the SiO and TiO layers is obtained by the method according to the invention. As compared to this, the shear stability of natural-mica-based pigments is rather bad due to the layered structure thereof and the morphology of the metal oxide layer.
  • the thickness of both layers is easy to regulate, in particular as compared to the hydrolysis belt method (shrinking of the deposited layer), and the color can be influenced in this way, with the thickness of the SiO layer influencing the color even stronger than the thickness of the TiO layer.
  • the backing in keeping with the invention, provision can be made for the backing to be enclosed on both sides by metal oxide layers of varying thickness (asymmetric layer structure).
  • asymmetric layer structure cannot be obtained by wet chemical processes.
  • the pigments when they are worked into paint and when an object is painted, will be located substantially parallel to the painted surface, varying thickness of the metal oxide layers will result in that, randomly distributed, either the thicker or thinner metal oxide layer is on top, which helps create colors and paints of novel interference effects.
  • another metal layer in particular an aluminum layer
  • a comparatively thin silicon oxide layer may be vapor-deposited as a protective layer on the aluminum layer.
  • a metal oxide layer and the backing layer are followed by a metal layer, a silicon oxide layer and another metal oxide layer, the metal layer being aluminum, chromium, gold, copper, silver or the like.
  • the metal oxide layer and the backing are followed by a metal layer, the metal again being aluminum, chromium, gold, copper, silver or the like.
  • the thickness of the backing preferably ranges between 20 and 1000 nm
  • the thickness of the metal oxide layer preferably ranges between 20 and 500 nm and that of the metal layer preferably between 40 and 60 nm.
  • the above-specified pigments according to the invention may have further layers on their surface, for example for increased weathering resistance. These layers can be applied by wet chemical or PVD processes (“inline”).
  • Suitable substances may be selected from the group of oxides and/or oxyhydrates and/or hydroxides of aluminum, silicon, zirconium, phosphor, boron, zinc, cerium, manganese, chromium, molybdenum, iron and tin.
  • the mentioned stabilizing substances may also be incorporated as a doping agent in the outermost layers.
  • a backing is produced by vacuum evaporation coating of a circulating metal belt; and that, after parting from the substrate, the backing particles thus produced are comminuted to a desired size, these backing particles then being equipped with another layer by wet coating.
  • the backing may consist in particular of silicon oxide, silicate, boron oxide, borates, aluminum oxide, aluminates, titanium boride or mixtures thereof.
  • the layers applied by wet chemical deposition may advantageously consist of oxides of the metals zirconium, chromium, titanium, iron, zinc, oxide hydrates of these metals, ferrotitanates, titanium suboxides or mixtures thereof, it being possible to reduce the metal oxides.
  • additional coatings may be applied for light stabilization and weathering resistance.
  • Another embodiment of the method according to the invention relates to the manufacture of single-layer nacreous pigments, wherein—apart from light stabilization and weathering resistance coatings that might be provided—a single, optically active layer of titanium oxide, iron oxide, titanium suboxides, titanium oxinitrides, molybdenum sulfide or ferrotitanium oxide is vacuum-deposited on a circulating metal belt.
  • Such single-layer structures preferably have an optically active layer of a thickness in the order of magnitude of 20 to 500 nm, preferably 40 to 100 nm. These single-layer structures excel in color brightness and purity. Putting them into practice has so far failed due to lacking shear stability, which can however be obtained by the process according to the invention.
  • Another embodiment of the method according to the invention relates to the manufacture of nacreous pigments from a metal oxide layer, in particular a titanium oxide layer, a metal layer and another metal oxide layer, in particular a titanium oxide layer, by vacuum evaporation coating on a circulating metal belt.
  • the metal may be aluminum, chromium, gold, copper, silver or the like.
  • a release coat may be applied, consisting of a paint, a salt, a salty compound or an organic material. Precipitation of this release coat may for instance take place by painting or evaporation.
  • the invention also relates to a nacreous pigment manufactured in accordance with one of the described methods as well as to paints, lacquers, cosmetics and plastics that comprise these nacreous pigments, and the use of these nacreous pigments for the production of paints, lacquers, cosmetics and plastics.
  • a release layer of a water soluble salt that is indecomposably high-vacuum evaporable is applied by vacuum (10 ⁇ 4 mbar) evaporation coating on a circulating metal belt, which is followed by a TiO layer, an SiO layer and another TiO layer.
  • the belt circulation speed is 2 m/s
  • the temperature of the TiO sources is 2200° C.
  • the distance of the evaporation sources from each other is 17 cm.
  • the optical thickness of the SiO layer is 202 nm, that of the TiO layers 198 nm.
  • the film After being parted from the metal belt in a water bath, the film is stirred by a high-speed stirrer and comminuted into pigment particles of a size of 1 to 100 ⁇ m.
  • the powder obtained has a blue color.
  • a release layer of a water soluble salt that is indecomposably high-vacuum evaporable is applied by vacuum (10 ⁇ 4 mbar) evaporation coating on a circulating metal belt, which is followed by a TiO layer, an aluminum layer and another TiO layer.
  • the belt circulation speed is 2 m/s
  • the temperature of the TiO sources is 2200° C.
  • the distance of the evaporation sources from each other is 17 cm.
  • the optical thickness of the aluminum layer is 245 nm, that of the TiO layers 603 nm.
  • the film After being parted from the metal belt in a water bath, the film is stirred by a high-speed stirrer and comminuted into pigment particles of a size of 1 to 100 ⁇ m.
  • the powder obtained has a light blue color of metallic character and nacreous luster.
  • a release layer of a water soluble salt that is indecomposably high-vacuum evaporable is applied by vacuum (10 ⁇ 4 mbar) evaporation coating on a circulating metal belt, which is followed by a TiO layer.
  • the belt circulation speed is 2 m/s
  • the temperature of the TiO sources is 2200° C.
  • the optical thickness of the TiO layer is 500 nm.
  • the film After being parted from the metal belt in a water bath, the film is stirred by a high-speed stirrer and comminuted into pigment particles of a size of 1 to 100 ⁇ m.
  • the powder obtained has a reddish yellow color.
  • a release layer of a water soluble salt that is indecomposably high-vacuum evaporable is applied by vacuum (10 ⁇ 4 mbar) evaporation coating on a circulating metal belt, which is followed by an SiO layer.
  • the belt circulation speed is 2 m/s, the temperature of the SiO source is 1450° C.
  • the optical thickness of the SiO layer is 200 nm.
  • the film After being parted from the metal belt in a water bath, the film is stirred by a high-speed stirrer and comminuted into pigment particles of a size of 1 to 100 ⁇ m.
  • the powder obtained is coated in a known manner with titanium dioxide by wet chemical treatment.

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US20050013934A1 (en) * 2003-06-17 2005-01-20 Rong Xiong Process for the preparation of a pigment comprising a core material and at least one dielectric layer
US20050090583A1 (en) * 2002-03-11 2005-04-28 Patrice Bujard Gloss pigments having high colour saturation
US20050161678A1 (en) * 2002-02-18 2005-07-28 Hilmar Weinert Methods of producing plane-parallel structures of silicon suboxide, silicon dioxide and/or silicon carbide, plane-parallel structures obtainable by such methods, and the use thereof
US20050252410A1 (en) * 2002-06-18 2005-11-17 Patrice Bujard Plane-parallel structures of silicon/silicon oxide
US20060027139A1 (en) * 2002-11-21 2006-02-09 Patrice Bujard Optically variable pigments having an asymmetrical layer structure
US20060042507A1 (en) * 2002-10-16 2006-03-02 Patrice Bujard Interference pigments on the basis of silicon oxides
US20060050115A1 (en) * 2002-10-17 2006-03-09 Patrice Bujard Process for dyeing or printing textile fibre materials with gloss pigments
US20080134940A1 (en) * 2005-02-02 2008-06-12 Ian Robert Wheeler Printing Process for Preparing Particulate Products
US20090145332A1 (en) * 2005-08-18 2009-06-11 Dunwilco (1198) Limted British Body Corporate Process
US7594962B2 (en) 2003-01-17 2009-09-29 Ciba Specialty Chemicals Corporation Process for the production of porous inorganic materials or a matrix material containing nanoparticles
US20090311437A1 (en) * 2006-07-17 2009-12-17 Dunwilco (1198) Limited Process
US20110107795A1 (en) * 2004-05-28 2011-05-12 Ngk Insulators, Ltd. Method of coloring surface of zirconium-based metallic glass component
US20110217551A1 (en) * 2005-08-12 2011-09-08 Dunwilco (1198) Limited Process for producing metal flakes
US9168394B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9168393B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9168209B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9320687B2 (en) 2013-03-13 2016-04-26 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
CN115260904A (zh) * 2021-04-30 2022-11-01 维达力实业（赤壁）有限公司 闪钻加硬涂料及其制备方法和应用

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DE102004049203A1 (de) * 2004-10-08 2006-04-20 Merck Patent Gmbh Effektpigmente auf Basis dünner SiO2-Plättchen
EP1904586B1 (en) 2005-06-22 2016-11-23 Basf Se Interference pigments on the basis of glass flakes
US20070134177A1 (en) * 2005-10-06 2007-06-14 Zimmermann Curtis J Effect Materials
JP4931054B2 (ja) * 2006-09-27 2012-05-16 株式会社アルバック 薄膜顔料の製造方法
US9631064B2 (en) * 2012-04-19 2017-04-25 Basf Se Process for preparing an effect pigment
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US20050161678A1 (en) * 2002-02-18 2005-07-28 Hilmar Weinert Methods of producing plane-parallel structures of silicon suboxide, silicon dioxide and/or silicon carbide, plane-parallel structures obtainable by such methods, and the use thereof
US7256425B2 (en) 2002-02-18 2007-08-14 Ciba Specialty Chemicals Corporation Methods of producing plane-parallel structures of silicon suboxide, silicon dioxide and/or silicon carbide, plane-parallel structures obtainable by such methods, and the use thereof
US7223472B2 (en) 2002-03-11 2007-05-29 Ciba Specialty Chemicals Corporation Gloss pigments having high colour saturation
US20050090583A1 (en) * 2002-03-11 2005-04-28 Patrice Bujard Gloss pigments having high colour saturation
US7273522B2 (en) 2002-06-18 2007-09-25 Ciba Specialty Chemicals Corporation Plane-parallel structures of silicon/silicon oxide
US20050252410A1 (en) * 2002-06-18 2005-11-17 Patrice Bujard Plane-parallel structures of silicon/silicon oxide
US20060042507A1 (en) * 2002-10-16 2006-03-02 Patrice Bujard Interference pigments on the basis of silicon oxides
US7959727B2 (en) 2002-10-16 2011-06-14 Basf Se Interference pigments on the basis of silicon oxides
US7517404B2 (en) 2002-10-16 2009-04-14 Ciba Specialty Chemicals Corporation Interference pigments on the basis of silicon oxides
US20090169499A1 (en) * 2002-10-16 2009-07-02 Patrice Bujard Interference pigments on the basis of silicon oxides
US20060050115A1 (en) * 2002-10-17 2006-03-09 Patrice Bujard Process for dyeing or printing textile fibre materials with gloss pigments
US20060027139A1 (en) * 2002-11-21 2006-02-09 Patrice Bujard Optically variable pigments having an asymmetrical layer structure
US7374609B2 (en) 2002-11-21 2008-05-20 Ciba Specialty Chemicals Corporation Optically variable pigments having an asymmetrical layer structure
US20100003520A1 (en) * 2003-01-17 2010-01-07 Patrice Bujard Porous inorganic materials of silcon and oxygen
US8177901B2 (en) 2003-01-17 2012-05-15 BASF SE Ludwigshafen Porous inorganic materials of silcon and oxygen
US7594962B2 (en) 2003-01-17 2009-09-29 Ciba Specialty Chemicals Corporation Process for the production of porous inorganic materials or a matrix material containing nanoparticles
JP2006527649A (ja) * 2003-06-17 2006-12-07 チバ　スペシャルティ　ケミカルズ　ホールディング　インコーポレーテッド マイクロ波付着による金属酸化物コーティド有機材料の製造方法
US20040265507A1 (en) * 2003-06-17 2004-12-30 Rong Xiong Process for the preparation of metal oxide coated organic material by microwave deposition
US7459182B2 (en) 2003-06-17 2008-12-02 Ciba Specialty Chemicals Corporation Process for the preparation of metal oxide coated organic material by microwave deposition
JP4908204B2 (ja) * 2003-06-17 2012-04-04 チバ ホールディング インコーポレーテッド マイクロ波付着による金属酸化物コーティド有機材料の製造方法
KR101125084B1 (ko) 2003-06-17 2012-03-21 시바 홀딩 인크 극초단파 증착에 의한 금속 산화물 피복된 유기 재료의제조방법
WO2004111298A1 (en) * 2003-06-17 2004-12-23 Ciba Specialty Chemicals Holding Inc. Process for the preparation of metal oxide coated organic material by microwave deposition
CN1809654B (zh) * 2003-06-17 2010-12-29 西巴特殊化学品控股有限公司 通过微波沉积制备金属氧化物涂布的有机材料的方法
US20050013934A1 (en) * 2003-06-17 2005-01-20 Rong Xiong Process for the preparation of a pigment comprising a core material and at least one dielectric layer
US20110107795A1 (en) * 2004-05-28 2011-05-12 Ngk Insulators, Ltd. Method of coloring surface of zirconium-based metallic glass component
US8865253B2 (en) * 2004-05-28 2014-10-21 Ngk Insulators, Ltd. Method of coloring surface of zirconium-based metallic glass component
US20080134940A1 (en) * 2005-02-02 2008-06-12 Ian Robert Wheeler Printing Process for Preparing Particulate Products
US20110217551A1 (en) * 2005-08-12 2011-09-08 Dunwilco (1198) Limited Process for producing metal flakes
US8016909B2 (en) 2005-08-12 2011-09-13 Dunwilco (1198) Limited Process for producing metal flakes
US20090145332A1 (en) * 2005-08-18 2009-06-11 Dunwilco (1198) Limted British Body Corporate Process
US20090311437A1 (en) * 2006-07-17 2009-12-17 Dunwilco (1198) Limited Process
US9168394B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9168393B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9168209B2 (en) 2013-03-13 2015-10-27 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
US9320687B2 (en) 2013-03-13 2016-04-26 Johnson & Johnson Consumer Inc. Pigmented skin-care compositions
CN115260904A (zh) * 2021-04-30 2022-11-01 维达力实业（赤壁）有限公司 闪钻加硬涂料及其制备方法和应用

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US20040261661A1 (en) 2004-12-30
EP1266977A2 (de) 2002-12-18
US7217318B2 (en) 2007-05-15
WO2001057287A1 (de) 2001-08-09
DE10004888A1 (de) 2001-08-09
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EP1266977B1 (de) 2005-05-25
AU2852301A (en) 2001-08-14
AU781222B2 (en) 2005-05-12

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