EP1559810A2 - Process for the preparation of a ceramic protective layer - Google Patents

Process for the preparation of a ceramic protective layer Download PDF

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Publication number
EP1559810A2
EP1559810A2 EP04028924A EP04028924A EP1559810A2 EP 1559810 A2 EP1559810 A2 EP 1559810A2 EP 04028924 A EP04028924 A EP 04028924A EP 04028924 A EP04028924 A EP 04028924A EP 1559810 A2 EP1559810 A2 EP 1559810A2
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European Patent Office
Prior art keywords
substrate
ceramic
solution
halide
metallic
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EP04028924A
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German (de)
French (fr)
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EP1559810A3 (en
Inventor
Frank Dr. Schneider
Wilfried Hoeger
Harald Arlt
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    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D5/00—Coating with enamels or vitreous layers
    • C23D5/02—Coating with enamels or vitreous layers by wet methods

Definitions

  • the invention relates to a method for applying a ceramic layer metallic or metallized surfaces.
  • a known method for producing such layers is the sol-gel method, in which a solution with microparticles, for example a mixture of Zirconium and silica prepared and to form a gel phase on a Substrate is applied and dried.
  • the object of the present invention is to provide a simple method without To offer heat treatment with the UV-resistant, as well as scratch-resistant and also under deformation, firmly adhering coatings can be produced.
  • FIG. 2a the structure of an optical glass is shown having a very low coefficient of friction / friction factor.
  • the coating 4 is applied to the metallised surface of a bearing metal.
  • FIGS. 3 to 5 show AFM images of layers which according to the invention have been provided with a zirconia wet coating according to the invention.
  • FIG. 3 shows the untreated quartz glass surface. After metallization receives by smoothing of concentration and reaction time smooth, for optical Applications suitable coatings (see Fig. 4) to spherical for friction-bearing coatings suitable surface structures (see Fig. 5).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

Die Erfindung betrifft ein Verfahren zur Aufbringung einer Keramikschicht auf metallische oder metallisierte Oberflächen eines Substrates, das dadurch gekennzeichnet ist, dass ein mit einem Halogenid gelöstes Metallalkoxid in Gegenwart einer Sauerstoffquelle auf die Oberfläche des Substrates aufgetragen und getrocknet wird. Die Erfindung betrifft ferner ein keramikbeschichtetes Substrat, das aus einem optischen Glas mit einer metallisierten Oberfläche besteht.

Figure 00000001
The invention relates to a method for applying a ceramic layer to metallic or metallized surfaces of a substrate, which is characterized in that a dissolved with a halide metal alkoxide is applied in the presence of an oxygen source on the surface of the substrate and dried. The invention further relates to a ceramic-coated substrate consisting of an optical glass with a metallized surface.
Figure 00000001

Description

Die Erfindung betrifft ein Verfahren zur Aufbringung einer Keramikschicht auf metallische oder metallisierte Oberflächen.The invention relates to a method for applying a ceramic layer metallic or metallized surfaces.

Ein bekanntes Verfahren zur Herstellung derartiger Schichten ist das Sol-Gel-Verfahren, bei dem eine Lösung mit Mikropartikeln, beispielsweise einem Gemisch aus Zirkon- und Siliziumoxid hergestellt und unter Ausbildung einer Gelphase auf ein Substrat aufgebracht und getrocknet wird. Zur Erzeugung einer harten und kratzfesten Schicht ist ein Tempern bei erhöhter Temperatur erforderlich. üblicherweise werden dabei Temperaturen zwischen 150 und 400°C angewendet ([2.]).A known method for producing such layers is the sol-gel method, in which a solution with microparticles, for example a mixture of Zirconium and silica prepared and to form a gel phase on a Substrate is applied and dried. To create a hard and scratch-resistant Layer is a tempering at elevated temperature required. usually become used temperatures between 150 and 400 ° C ([2.]).

Aufgabe der vorliegenden Erfindung ist es, ein einfaches Verfahren ohne Wärmebehandlung anzubieten mit dem UV-beständige, sowie kratzfeste und auch unter Verformung fest anhaftende Beschichtungen hergestellt werden können.The object of the present invention is to provide a simple method without To offer heat treatment with the UV-resistant, as well as scratch-resistant and also under deformation, firmly adhering coatings can be produced.

Diese Aufgabe wird erfindungsgemäß mit den in den Patentansprüchen angegebenen Merkmale gelöst. Es hat sich gezeigt, dass mit einer einfachen Nassbeschichtung bei Normaltemperatur in kurzer Behandlungszeit eine sehr haftfeste, stoß- und kratzunempfindliche Beschichtung aus hochwertiger Keramik hergestellt werden kann.This object is achieved according to the invention with the specified in the claims Characteristics solved. It has been shown that with a simple wet coating at Normal temperature in a short treatment time a very adherent, shock and Scratch-resistant coating can be made of high quality ceramic.

Im folgenden wird die Erfindung anhand eines Ausführungsbeispiels erläutert. Es zeigen:

Fig. 1:
Darstellung des Verfahrensablaufes
Fig. 2a,b:
Querschnitte durch erfindungsgemäß aufgebaute, beschichtete Substrate (Prinzipbilder)
Fig. 3:
Kraftmikroskop (AFM)-Aufnahme einer Quarzglas-Oberfläche
Fig.4:
AFM-Aufnahme eines beschichteten Quarzglases analog zu Fig. 2b
Fig. 5:
AFM-Aufnahme eines beschichteten Quarzglases analog zu Fig.2a
In the following the invention will be explained with reference to an embodiment. Show it:
Fig. 1:
Presentation of the procedure
Fig. 2a, b:
Cross sections through coated substrates constructed according to the invention (schematic diagrams)
3:
Force microscope (AFM) image of a quartz glass surface
Figure 4:
AFM image of a coated quartz glass analogous to FIG. 2b
Fig. 5:
AFM image of a coated quartz glass analogous to FIG. 2a

Der Verfahrensablauf zur Herstellung einer erfindungsgemäßen Keramikschicht ist den Prinzipbildern in Figuren 1 und 2 zu entnehmen. Fig.1 zeigt die folgenden Verfahrensschritte:

  • 1.1 Oberfläche beizen
  • 1.2 Halogenidlösung/Metallalkoxid herstellen
  • 1.3 Oberfläche behandeln
  • 1.4 Peroxid zugeben
  • 1.5 Oberfläche trocknen
    • The process sequence for the production of a ceramic layer according to the invention can be found in the schematic diagrams in FIGS. 1 and 2. 1 shows the following method steps:
  • 1.1 Stain the surface
  • 1.2 produce halide solution / metal alkoxide
  • 1.3 Treat surface
  • 1.4 Add peroxide
  • 1.5 Dry the surface

    • Aus der Darstellung nach Fig.2a ist der Aufbau eines optischen Glases ersichtlich.Mit 1 ist eine transparente Keramikschicht, mit 2 eine Metallschicht und mit 3 das optische Glas bezeichnet.Alternativ hierzu zeigt Fig.2b die Situation bei einer Reib-Lager-Beschichtung 4, die einen sehr niedrigen Reibwert/Reibfaktor aufweist.Die Beschichtung 4 ist auf der metallisierten Oberfläche eines Lagermetalls aufgebracht.
    Die Figuren 3 bis 5 zeigen AFM-Aufnahmen von Schichten, die entsprechend den Prinzipbildern erfindungsgemäß mit einer Nassbeschichtung aus Zirkondioxid versehen wurden.    With reference to FIG. 2a, the structure of an optical glass is shown having a very low coefficient of friction / friction factor. The coating 4 is applied to the metallised surface of a bearing metal.
    FIGS. 3 to 5 show AFM images of layers which according to the invention have been provided with a zirconia wet coating according to the invention.

    Figur 3 zeigt die unbehandelte Quarzglasoberfläche. Nach der Metallisierung erhält man durch Variation von Konzentration und Reaktionszeit glatte, für optische Anwendungen geeignete Beschichtungen (s. Fig. 4) bis hin zu kugelförmigen für Reib-Lager-Beschichtungen geeignete Oberflächenstrukturen (s. Fig. 5).FIG. 3 shows the untreated quartz glass surface. After metallization receives by smoothing of concentration and reaction time smooth, for optical Applications suitable coatings (see Fig. 4) to spherical for friction-bearing coatings suitable surface structures (see Fig. 5).

    Claims (10)

    Verfahren zur Aufbringung einer Keramikschicht auf metallische oder metallisierte Oberflächen eines Substrates, dadurch gekennzeichnet, dass ein mit einem Halogenid gelöstes Metallalkoxid in Gegenwart einer Sauerstoffquelle auf die Oberfläche des Substrates aufgetragen und getrocknet wird.A method for applying a ceramic layer to metallic or metallized surfaces of a substrate, characterized in that a dissolved with a halide metal alkoxide is applied in the presence of an oxygen source on the surface of the substrate and dried. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass vor Aufbringung der Lösung eine Beizbehandlung der metallischen oder metallisierten Oberfläche erfolgt.A method according to claim 1, characterized in that prior to application of the solution, a pickling treatment of the metallic or metallized surface. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass vor Aufbringung der Lösung die Oberfläche des Substrates oxidiert wird.A method according to claim 1 or 2, characterized in that prior to application of the solution, the surface of the substrate is oxidized. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Sauerstoffquelle ein Peroxid ist.Method according to one of the preceding claims, characterized in that the oxygen source is a peroxide. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das Metallalkoxid aus Zirkon- und/oder Titanalkoxid besteht.Method according to one of the preceding claims, characterized in that the metal alkoxide consists of zirconium and / or titanium alkoxide. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass als Halogenid eine Chlorid-Verbindung eingesetzt wird.Method according to one of the preceding claims, characterized in that a chloride compound is used as the halide. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass eine alkoholische Lösung des Halogenids verwendet wird und diese Lösung in einem Nassbeschichtungsverfahren aufgetragen wird.Method according to one of the preceding claims, characterized in that an alcoholic solution of the halide is used and this solution is applied in a wet coating process. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Nassbeschichtung durch Tauchen, Sprühen, Schleudern, Fluten oder durch Bedrucken erfolgt. Method according to one of the preceding claims, characterized in that the wet coating is carried out by dipping, spraying, spinning, flooding or by printing. Keramikbeschichtetes Substrat, hergestellt nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Keramikschicht aus einer transparenten glasartigen Phase besteht.Ceramic-coated substrate, produced according to one of the preceding claims, characterized in that the ceramic layer consists of a transparent vitreous phase. Keramikbeschichtetes Substrat nach Anspruch 9, dadurch gekennzeichnet, dass das Substrat aus einem optischen Glas mit einer metallisierten Oberfläche besteht.Ceramic coated substrate according to claim 9, characterized in that the substrate consists of an optical glass with a metallised surface.
    EP04028924A 2003-12-29 2004-12-07 Process for the preparation of a ceramic protective layer Withdrawn EP1559810A3 (en)

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    Cited By (3)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    WO2007050501A3 (en) * 2005-10-24 2007-08-02 Crg Chemical Inc Polymeric organometallic films
    US7740940B2 (en) 2006-11-15 2010-06-22 Aculon, Inc. Coated substrates, organometallic films and methods for applying organometallic films to substrates
    US8048487B2 (en) * 2006-11-15 2011-11-01 Aculon, Inc. Organometallic films, methods for applying organometallic films to substrates and substrates coated with such films

    Family Cites Families (4)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    JPH01132770A (en) * 1987-08-20 1989-05-25 Central Glass Co Ltd Composition for titanium-containing oxide film and formation of said film
    JP3251167B2 (en) * 1996-02-09 2002-01-28 日本パーカライジング株式会社 Titanium oxide-based ceramic paint and method for producing the same
    DE19736925A1 (en) * 1996-08-26 1998-03-05 Central Glass Co Ltd Hydrophilic film and method for producing the same on a substrate
    TW533440B (en) * 2000-12-19 2003-05-21 Toho Titanium Co Ltd Method for forming titanium oxide film and titanium electrolytic capacitor

    Cited By (6)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    WO2007050501A3 (en) * 2005-10-24 2007-08-02 Crg Chemical Inc Polymeric organometallic films
    US7989069B2 (en) 2005-10-24 2011-08-02 Aculon, Inc. Polymeric organometallic films
    US7740940B2 (en) 2006-11-15 2010-06-22 Aculon, Inc. Coated substrates, organometallic films and methods for applying organometallic films to substrates
    US7901777B2 (en) 2006-11-15 2011-03-08 Aculon, Inc. Coated substrates, organometallic films and methods for applying organometallic films to substrates
    US8048487B2 (en) * 2006-11-15 2011-11-01 Aculon, Inc. Organometallic films, methods for applying organometallic films to substrates and substrates coated with such films
    US8337985B2 (en) 2006-11-15 2012-12-25 Aculon, Inc. Coated substrates, organometallic films and methods for applying organometallic films to substrates

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