WO1994016022A1 - Method of producing gold- or silver-coloured pigments or pigments of other colours - Google Patents

Method of producing gold- or silver-coloured pigments or pigments of other colours Download PDF

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Publication number
WO1994016022A1
WO1994016022A1 PCT/DE1994/000024 DE9400024W WO9416022A1 WO 1994016022 A1 WO1994016022 A1 WO 1994016022A1 DE 9400024 W DE9400024 W DE 9400024W WO 9416022 A1 WO9416022 A1 WO 9416022A1
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Prior art keywords
pigments
titanium
hafnium
zirconium
nitrides
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PCT/DE1994/000024
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German (de)
French (fr)
Inventor
Hans Joachim Bock
Siegfried Sattelberger
Bernd Friedrich
Original Assignee
Carl Schlenk Aktiengesellschaft
GfE Gesellschaft für Elektrometallurgie mbH
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Publication of WO1994016022A1 publication Critical patent/WO1994016022A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0602—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with two or more other elements chosen from metals, silicon or boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
    • C01B21/0768—After-treatment, e.g. grinding, purification
    • 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
    • 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
    • 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • 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
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Definitions

  • the invention relates to a method for producing gold, silver or other colored pigments according to the preamble of claim 1.
  • metal pigments in particular made of aluminum or brass, in the production of paints and lacquers with gold or silver-colored effects. Different gold tones can be set by the zinc content in the brass. Other shades can also be achieved through special treatment steps.
  • Products are also known which achieve a gold color by coloring aluminum pigments.
  • DE-A-34 43 622 discloses the use of titanium oxynitride in powder form as a non-toxic pigment, the color of which, depending on the composition, ranges from black to brownish and pupar black to blue black. Pigments with lighter shades, especially gold or silver-colored pigments, cannot be produced from this material.
  • titanium nitride is known as a very hard material for the production of protective surface layers on machine bearings, roller bearings and the like, and also for lining reaction vessels, in particular for liquid metals such as aluminum, copper and iron.
  • This titanium nitride consists of gold-yellow crystals, is insoluble in water, is resistant to many acids and has a Mohs hardness of 8 to 9.
  • the invention has for its object to provide a process for the production of non-toxic, biocompatible gold, silver or other colored pigments with high gloss and reflectivity.
  • a plastic film with a separating layer which is soluble in organic solvents is used as the carrier.
  • the nitride layer on platelet-shaped parts with an average diameter of 0.8 microns to 100 microns, preferably from 5 microns to 50 microns, and with a thickness of 0.02 microns to 2 microns , preferably from 0.1 ⁇ m to 1 ⁇ m.
  • the surface of the platelet-shaped pigments is smoothed in a subsequent polishing step.
  • nitrides are advantageously used as pigments in solvent-based or water-dilutable lacquers or Colors, incorporated in cosmetics or in plastics.
  • biocompatible pigments are produced and used which are stable both against air and water and against a large number of chemical compounds and maintain these properties even at higher temperatures without an additional processing step.
  • these pigments are preferably used in paints and lacquers which are used for printing packaging for foodstuffs. These pigments are also suitable for use in the cosmetics industry and for coloring plastics, where temperature and chemical stability are required.
  • titanium alloy nitrides with a platelet-shaped structure are used, the individual nitride platelets preferably having a medium one Have a diameter of 5 ⁇ m to 50 ⁇ m and a thickness of 0.1 ⁇ m to 1 ⁇ m.
  • nitrides can be used as pigments in solvent-based or water-dilutable lacquers or paints, in cosmetics or in plastics.
  • Such platelet-shaped titanium alloy nitrides are produced by the process according to the invention as follows:
  • a titanium nitride layer is evaporated in vacuo onto a support, for example onto a plastic film, to which a separating layer soluble in organic solvents has previously been applied.
  • This titanium nitride layer is a very hard layer which, depending on the duration of the process, reaches a thickness corresponding to the desired platelet-like structure.
  • the separating layer is then dissolved with the solvent, so that the very hard titanium nitride layer can easily be detached from the support and comminuted to the desired average platelet diameter, which is easily possible with the small thickness.
  • the surface can be smoothed in a subsequent polishing step.
  • Films made of polyethylene terephthalate, polyacetate or the like are particularly suitable as supports for the nitride layer to be evaporated.
  • Materials made of or on the are particularly suitable as the separating layer soluble in organic solvents Base of polyvinyl chloride, polystyrene, methyl methacrylate or the like ..
  • pigments can also be produced in a corresponding manner from titanium oxide or titanium alloy nitride layers, from zirconium, zirconium oxide or zirconium alloy nitride layers or from hafnium, hafnium oxi or hafnium alloy nitride layers.

Abstract

The invention concerns a method of producing gold-coloured or silver-coloured pigments or pigments of other colours, the aim being to produce non-toxic, environmentally compatible pigments of these kinds. This aim is achieved by evaporating in a vacuum a titanium nitride, titanium oxynitride or titanium-alloy nitride film, a zirconium nitride, zirconium oxynitride or zirconium-alloy nitride film or a hafnium nitride, hafnium oxynitride or hafnium-alloy nitride film on to a substrate on which a solvent-soluble coating-release film has previously been applied. The nitride film is subsequently detached by dissolving the coating-release film, and the nitride film reduced to the particle size required for the pigment.

Description

Verfahren zur Herstellung von gold-, silber- oder andersfarbigen Piσmenten Process for the production of gold, silver or other colored pigments
Die Erfindung bezieht sich auf ein Verfahren zur Herstellung von gold-, silber- oder andersfarbigen Pigmenten nach dem Oberbegriff des Anspruches 1.The invention relates to a method for producing gold, silver or other colored pigments according to the preamble of claim 1.
Es ist bekannt, bei der Herstellung von Farben und Lacken mit gold- oder silberfarbigen Effekten Metallpigmente, insbesondere aus Aluminium oder Messing, einzusetzen. Dabei können verschiedene Goldtöne durch den Zinkgehalt im Messing eingestellt werden. Durch spezielle Behandlungsschritte können auch andere Farbtöne erzielt werden.It is known to use metal pigments, in particular made of aluminum or brass, in the production of paints and lacquers with gold or silver-colored effects. Different gold tones can be set by the zinc content in the brass. Other shades can also be achieved through special treatment steps.
Bei diesen Pigmenten werden ein großes Reflexionsvermögen und hoher Glanz durch eine plättchenförmige Struktur der Pigmente erzielt, die jedoch nur erzeugt werden kann, wenn die Ausgangsstoffe in gewissem Maße verformbar sind. Das führt andererseits dazu, daß diese Stoffe nicht sehr hart sein dürfen, so daß ihre Verwendbarkeit stark eingeschränkt ist.With these pigments, a high reflectivity and high gloss are achieved by a platelet-shaped structure of the pigments, which, however, can only be produced if the starting materials are deformable to a certain extent. On the other hand, this means that these substances must not be very hard, so that their usability is severely restricted.
Es sind auch Produkte bekannt, die eine Goldfarbe durch Einfärben von Aluminiumpigmenten erzielen.Products are also known which achieve a gold color by coloring aluminum pigments.
Neuere Entwicklungen basieren auf beschichteten Glimmer¬ pigmenten oder auf mit Eisenoxid beschichteten Aluminium- pigmenten, wobei der Farbeindruck auf Interferenzer¬ scheinungen beruht.Recent developments are based on coated mica pigments or on aluminum oxide coated with iron oxide. pigments, the color impression being based on interference phenomena.
Diese bekannten Pigmente sind entweder nicht sehr stabil, insbesondere bei höheren Temperaturen, oder sie sind wegen ihrer toxischen Eigenschaften nicht überall, insbesondere nicht in der Lebensmittel- oder Kosmetikbranche, einsetzbar.These known pigments are either not very stable, especially at higher temperatures, or because of their toxic properties, they cannot be used everywhere, especially not in the food or cosmetics industry.
Aus der DE-A- 34 43 622 ist die Verwendung von Titan- oxinitrid in Pulverform als nichttoxisches Pigment bekannt, dessen Farbgebung je nach Zusammensetzung von schwarz über bräunlich- und pupurschwarz bis zu blauschwarz reicht. Pigmente mit helleren Farbtönen, insbesondere gold- oder silberfarbige Pigmente, sind aus diesem Material nicht herstellbar.DE-A-34 43 622 discloses the use of titanium oxynitride in powder form as a non-toxic pigment, the color of which, depending on the composition, ranges from black to brownish and pupar black to blue black. Pigments with lighter shades, especially gold or silver-colored pigments, cannot be produced from this material.
Andere Literaturstellen, die sich mit Titannitrid befassen, offenbaren lediglich die Verwendung als harte Oberflächen¬ schichten. Die Verwendung als Pigment ist diesen Schriften nicht zu entnehmen, wie nachfolgende Beispiele zeigen.Other references that deal with titanium nitride only disclose the use as hard surface layers. The use as a pigment is not apparent from these documents, as the following examples show.
Aus Rö pps-Chemielexikon 1977 ist Titannitrid als ein sehr harter Stoff zur Herstellung von schützenden Oberflächen¬ schichten auf Maschinenlagern, Wälzlagern und dergleichen, ferner zur Auskleidung von Reaktionsbehältern, insbesondere für flüssige Metalle, wie Aluminium, Kupfer und Eisen, bekannt. Dieses Titannitrid besteht aus goldgelben Kristallen, ist im Wasser unlöslich, ist beständig gegen viele Säuren und hat die Mohshärte 8 bis 9.From Rö pps chemistry lexicon 1977 titanium nitride is known as a very hard material for the production of protective surface layers on machine bearings, roller bearings and the like, and also for lining reaction vessels, in particular for liquid metals such as aluminum, copper and iron. This titanium nitride consists of gold-yellow crystals, is insoluble in water, is resistant to many acids and has a Mohs hardness of 8 to 9.
Aus der DE-C- 963 151 ist ein Verfahren zur Herstellung von feinverteiltem Titannitrid bekannt, das in der metallurgischen Technik zur Herstellung von Gußstücken großer Festigkeit und Härte verwendbar ist.From DE-C-963 151 a process for the production of finely divided titanium nitride is known, which in the metallurgical technology for the production of castings of great strength and hardness can be used.
Aus der DE-B- 1 160 831 ist ein weiteres Verfahren zur Herstellung von Titannitrid bekannt, das in äußerst feiner Verteilung anfällt und deshalb zur Herstellung von Form¬ körpern durch Pressen und anschließendes Sintern besonders geeignet ist.Another process for the production of titanium nitride is known from DE-B-1 160 831, which is obtained in an extremely fine distribution and is therefore particularly suitable for the production of moldings by pressing and subsequent sintering.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren für die Herstellung nichttoxischer, bioverträglicher gold-, silber- oder andersfarbiger Pigmente mit hohem Glanz und Reflexionsvermögen zu schaffen.The invention has for its object to provide a process for the production of non-toxic, biocompatible gold, silver or other colored pigments with high gloss and reflectivity.
Diese Aufgabe wird durch die Merkmale des Anspruches 1 gelöst.This object is solved by the features of claim 1.
Nach einer vorteilhaften Ausgestaltung der Erfindung wird als Träger eine Kunststoffolie mit einer in organischen Lösungsmitteln löslichen Trennschicht verwendet.According to an advantageous embodiment of the invention, a plastic film with a separating layer which is soluble in organic solvents is used as the carrier.
Nach einer weiteren vorteilhaften Ausgestaltung der Erfindung ist vorgesehen, daß die Nitridschicht auf plättchenförmige Teile mit einem mittleren Durchmesser von 0,8 μm bis 100 μm, vorzugsweise von 5 μm bis 50 μm, und mit einer Dicke von 0,02 μm um bis 2 μm, vorzugsweise von 0,1 μm bis 1 μm, zerkleinert wird.According to a further advantageous embodiment of the invention it is provided that the nitride layer on platelet-shaped parts with an average diameter of 0.8 microns to 100 microns, preferably from 5 microns to 50 microns, and with a thickness of 0.02 microns to 2 microns , preferably from 0.1 μm to 1 μm.
Nach einer weiteren Ausgestaltung der Erfindung wird die Oberfläche der plättchenförmigen Pigmente in einem anschließenden Polierschritt geglättet.According to a further embodiment of the invention, the surface of the platelet-shaped pigments is smoothed in a subsequent polishing step.
Schließlich werden mit Vorteil die Nitride als Pigmente in lösungsmittelhaltigen oder wasserverdünnbaren Lacken oder Farben, in Kosmetika oder in Kunststoffen eingebracht.Finally, the nitrides are advantageously used as pigments in solvent-based or water-dilutable lacquers or Colors, incorporated in cosmetics or in plastics.
Die mit der Erfindung erzielten Vorteile bestehen insbesondere darin, daß bioverträgliche Pigmente hergestellt und verwendet werden, die sowohl gegen Luft und Wasser als auch gegen eine Vielzahl von chemischen Verbindungen stabil sind und diese Eigenschaften auch bei höheren Temperaturen ohne zusätzlichen Bearbeitungsschritt beibehalten.The advantages achieved by the invention consist in particular in the fact that biocompatible pigments are produced and used which are stable both against air and water and against a large number of chemical compounds and maintain these properties even at higher temperatures without an additional processing step.
Wegen der Stabilität ihrer Verbindung eignen sich diese Pigmente hervorragend für die Verwendung in wasserver¬ dünnbaren Systemen.Because of the stability of their connection, these pigments are outstandingly suitable for use in water-thinnable systems.
Ferner werden diese Pigmente wegen ihrer besonderen Eigen¬ schaften bevorzugt in Farben und Lacken eingesetzt, die zum Bedrucken von Verpackungen für Lebensmittel verwendet werden. Ebenso geeignet sind diese Pigmente zum Einsatz in der Kosmetikbranche sowie zum Färben von Kunststoffen, bei denen Temperatur- und chemische Stabilität gefordert sind.Furthermore, because of their special properties, these pigments are preferably used in paints and lacquers which are used for printing packaging for foodstuffs. These pigments are also suitable for use in the cosmetics industry and for coloring plastics, where temperature and chemical stability are required.
Als besonderer Vorteil ist hervorzuheben, daß diese Pigmente absolut frei von Schwermetallen sind und somit den An¬ forderungen des Umweltschutzes voll gerecht werden.It should be emphasized as a particular advantage that these pigments are absolutely free of heavy metals and thus fully meet the requirements of environmental protection.
Ein Ausführungsbeispiel der Erfindung wird nachfolgend näher beschrieben.An embodiment of the invention is described in more detail below.
Zur Schaffung nichttoxischer, bioverträglicher gold-, silber- oder andersfarbiger Pigmente mit hohem Glanz und Reflexionsvermögen werden beispielsweise Titanlegierungs- nitride mit einer plättchenförmigen Struktur verwendet, wo¬ bei die einzelnen Nitridplättchen bevorzugt einen mittleren Durchmesser von 5 μm bis 50 μm und eine Dicke von 0,1 μm bis 1 μm haben.To create non-toxic, biocompatible gold, silver or other colored pigments with high gloss and reflectivity, for example titanium alloy nitrides with a platelet-shaped structure are used, the individual nitride platelets preferably having a medium one Have a diameter of 5 μm to 50 μm and a thickness of 0.1 μm to 1 μm.
Diese Nitride können als Pigmente in lösungs ittelhaltigen oder wasserverdünnbaren Lacken oder Farben, in Kosmetika oder in Kunststoffen eingesetzt werden.These nitrides can be used as pigments in solvent-based or water-dilutable lacquers or paints, in cosmetics or in plastics.
Die Herstellung derartiger plättchenförmiger Titan¬ legierungsnitride erfolgt nach dem erfindungsgemäßen Verfahren wie folgt:Such platelet-shaped titanium alloy nitrides are produced by the process according to the invention as follows:
Es wird eine Titannitridschicht im Vakuum auf einen Träger, beispielsweise auf eine Kunststoffolie, aufgedampft, auf die zuvor eine in organischen Lösungsmitteln lösliche Trenn¬ schicht aufgebracht worden ist. Diese Titannitridschicht ist eine sehr harte Schicht, die je nach Dauer des Prozesses eine der gewünschten plättchenförmigen Struktur entsprechende Dicke erreicht. Anschließend wird die Trenn¬ schicht mit dem Lösungsmittel aufgelöst, so daß die sehr harte Titannitridschicht leicht vom Träger abgelöst und auf den gewünschten mittleren Plättchendurchmesser zerkleinert werden kann, was bei der geringen Dicke problemlos möglich ist.A titanium nitride layer is evaporated in vacuo onto a support, for example onto a plastic film, to which a separating layer soluble in organic solvents has previously been applied. This titanium nitride layer is a very hard layer which, depending on the duration of the process, reaches a thickness corresponding to the desired platelet-like structure. The separating layer is then dissolved with the solvent, so that the very hard titanium nitride layer can easily be detached from the support and comminuted to the desired average platelet diameter, which is easily possible with the small thickness.
Zur Erhöhung des Reflexionsvermögens und des Glanzes der Pigmente kann deren Oberfläche in einem anschließenden Polierschritt geglättet werden.To increase the reflectivity and gloss of the pigments, the surface can be smoothed in a subsequent polishing step.
Als Träger für die aufzudampfende Nitridschicht eignen sich insbesondere Folien aus Polyathylen-Terephthalat, Polyazetat oder dgl..Films made of polyethylene terephthalate, polyacetate or the like are particularly suitable as supports for the nitride layer to be evaporated.
Als in organischen Lösungsmitteln lösliche Trennschicht eignen sich insbesondere Materialien aus oder auf der Basis von Polyvinyl-Chlorid, Polystyrol, Methyl-Methacrylat oder dgl..Materials made of or on the are particularly suitable as the separating layer soluble in organic solvents Base of polyvinyl chloride, polystyrene, methyl methacrylate or the like ..
Wie vorstehend beschrieben, lassen sich in entsprechender Weise auch Pigmente aus Titanoxi- oder Titanlegierungs- Nitridschichten, aus Zirkonium, Zirkoniumoxi- oder Zirkoniu legierungs-Nitridschichten oder aus Hafnium-, Hafniumoxi- oder Hafniumlegierungs-Nitridschichten herstellen. As described above, pigments can also be produced in a corresponding manner from titanium oxide or titanium alloy nitride layers, from zirconium, zirconium oxide or zirconium alloy nitride layers or from hafnium, hafnium oxi or hafnium alloy nitride layers.

Claims

Patentansprüche Claims
1. Verfahren zur Herstellung von Titan-, Titanoxi- oder Titanlegierungsnitriden, von Zirkonium-, Zirkoniumoxi- oder Zirkoniumlegierungsnitriden oder von Hafnium-, Hafniumoxi- oder Hafniumlegierungsnitriden zur Verwendung als nicht¬ toxische, bioverträgliche gold-, silber- oder andersfarbige Pigmente, dadurch gekennzeichnet, daß eine Titan-, Titanoxi- oder Titanlegierungs-Nitridschicht, eine Zirkonium-, Zirkoniumoxi- oder Zirkoniumlegierungs-Nitridschicht oder eine Hafnium-, Hafniumoxi- oder Hafniumlegierungs- Nitridschicht im Vakuum auf einen Träger aufgedampft wird, auf den zuvor eine in einem Lösungsmittel lösliche Trennschicht aufgebracht worden ist, und daß danach durch Auflösen der Trennschicht die Nitridschicht abgelöst und auf die gewünschte Pigmentgröße zerkleinert wird.1. A process for the preparation of titanium, titanium oxi or titanium alloy nitrides, of zirconium, zirconium oxi or zirconium alloy nitrides or of hafnium, hafnium oxi or hafnium alloy nitrides for use as non-toxic, biocompatible gold, silver or other colored pigments, characterized that a titanium, titanium oxi or titanium alloy nitride layer, a zirconium, zirconium oxi or zirconium alloy nitride layer or a hafnium, hafnium oxi or hafnium alloy nitride layer is evaporated in vacuo onto a support onto which a solvent-soluble layer is previously deposited Separating layer has been applied, and that the nitride layer is then detached and comminuted to the desired pigment size by dissolving the separating layer.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Träger eine Kunststoffolie mit einer in organischen Lösungsmitteln löslichen Trennschicht verwendet wird.2. The method according to claim 1, characterized in that a plastic film is used with a separating layer soluble in organic solvents as a carrier.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Nitridschicht auf plättchenformige Teile mit einem mittleren Durchmesser von 0,8 μm bis 100 μm, vorzugsweise von 5 μm bis 50 μm, und mit einer Dicke von 0,02 μm bis 2 μm, vorzugsweise von 0,1 μm bis 1 μm, zerkleinert wird. 3. The method according to claim 1 or 2, characterized in that the nitride layer on platelet-shaped parts with an average diameter of 0.8 microns to 100 microns, preferably from 5 microns to 50 microns, and with a thickness of 0.02 microns to 2 μm, preferably from 0.1 μm to 1 μm, is comminuted.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Oberfläche der plättchenförmigen Pigmente in einem anschließenden Polierschritt geglättet wird.4. The method according to any one of claims 1 to 3, characterized in that the surface of the platelet-shaped pigments is smoothed in a subsequent polishing step.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Nitride als Pigmente in lösungs- mittelhaltigen oder wasserverdunnbaren Lacken oder Farben eingebracht werden.5. The method according to any one of claims 1 to 4, characterized in that the nitrides are introduced as pigments in solvent-based or water-thinnable lacquers or paints.
6. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Nitride als Pigmente in Kosmetika eingebracht werden.6. The method according to any one of claims 1 to 4, characterized in that the nitrides are introduced as pigments in cosmetics.
7. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Nitride als Pigmente in Kunststoffen eingebracht werden. 7. The method according to any one of claims 1 to 4, characterized in that the nitrides are introduced as pigments in plastics.
PCT/DE1994/000024 1993-01-14 1994-01-12 Method of producing gold- or silver-coloured pigments or pigments of other colours WO1994016022A1 (en)

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DE4300720 1993-01-14

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EP0950619A1 (en) * 1998-04-18 1999-10-20 Kabushiki Kaisha Tsukioka Foil storage container and foil material stored in this container
WO2003046245A2 (en) * 2001-11-29 2003-06-05 Avery Dennison Corporation Process for making angstrom scale and high aspect functional platelets
US6863851B2 (en) 1998-10-23 2005-03-08 Avery Dennison Corporation Process for making angstrom scale and high aspect functional platelets

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US4168986A (en) * 1978-07-03 1979-09-25 Polaroid Corporation Method for preparing lamellar pigments
JPS58167409A (en) * 1982-03-26 1983-10-03 Yaskawa Electric Mfg Co Ltd Formation method of zirconium nitride film having golden color
JPS58219265A (en) * 1982-06-14 1983-12-20 Toyota Motor Corp Preparation of metallic luster pigment
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0950619A1 (en) * 1998-04-18 1999-10-20 Kabushiki Kaisha Tsukioka Foil storage container and foil material stored in this container
US6863851B2 (en) 1998-10-23 2005-03-08 Avery Dennison Corporation Process for making angstrom scale and high aspect functional platelets
US7820088B2 (en) 1998-10-23 2010-10-26 Avery Dennison Corporation Process for making angstrom scale and high aspect functional platelets
WO2003046245A2 (en) * 2001-11-29 2003-06-05 Avery Dennison Corporation Process for making angstrom scale and high aspect functional platelets
WO2003046245A3 (en) * 2001-11-29 2004-02-12 Avery Dennison Corp Process for making angstrom scale and high aspect functional platelets

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