DE3816495A1 - METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS - Google Patents

METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS

Info

Publication number
DE3816495A1
DE3816495A1 DE19883816495 DE3816495A DE3816495A1 DE 3816495 A1 DE3816495 A1 DE 3816495A1 DE 19883816495 DE19883816495 DE 19883816495 DE 3816495 A DE3816495 A DE 3816495A DE 3816495 A1 DE3816495 A1 DE 3816495A1
Authority
DE
Germany
Prior art keywords
titanium
nickel
heat treatment
fluoride
adhesive
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
DE19883816495
Other languages
German (de)
Inventor
Gerd Dipl Chem Dr Linka
Michael Marquardt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bayer Pharma AG
Original Assignee
Schering AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Schering AG filed Critical Schering AG
Priority to DE19883816495 priority Critical patent/DE3816495A1/en
Priority to EP89107902A priority patent/EP0341546A3/en
Priority to JP11524189A priority patent/JPH0270073A/en
Publication of DE3816495A1 publication Critical patent/DE3816495A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • 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
    • C23C18/16—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 by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites

Description

Die Erfindung betrifft ein Verfahren zur haftfesten Metallisierung von Titan oder Titanlegierungen durch außenstromlose Abscheidung einer Nickel-Phosphor- Legierung mit anschließender Wärmebehandlung zur Ausbildung von Nickel-Titan- Diffusionsschichten.The invention relates to a method for the adhesive metallization of titanium or titanium alloys by electroless deposition of a nickel-phosphorus Alloy with subsequent heat treatment to form nickel-titanium Diffusion layers.

Das Galvanisieren der genannten Werkstoffe ist schwierig, da die Oberfläche von einer Passivierungsschicht überzogen ist.The galvanizing of the materials mentioned is difficult because the surface of is coated with a passivation layer.

Um Titan oder Titanlegierungen haftfest zu metallisieren, muß die Passivie­ rungsschicht entfernt werden. Dies erfolgt in bekannter Weise mittels wäßriger Lösungen von Flußsäure oder fluoridhaltigen Säuren. Ist die Passivierungs­ schicht von der Oberfläche entfernt, können Titan oder Titanlegierungen galva­ nisch beschichtet werden.To metallize titanium or titanium alloys firmly, the passivie be removed. This is done in a known manner using aqueous Solutions of hydrofluoric acid or acids containing fluoride. Is the passivation layer away from the surface, titanium or titanium alloys can galva nically coated.

In der DE-OS 36 22 032 wird dies mit einem Nickelsulfamatelektrolyten bei 5 A/dm2 und 55°C für 10 Min. versucht. Es gelingt jedoch nicht, aus derartigen Elektrolyten Schichten mit ausreichender Haftung abzuscheiden, da die Eigen­ spannungen der Schichten im Zugspannungsbereich liegen. In der DE 33 21 231 werden außenstromlos abgeschiedene Nickelschichten auf Oberflächen von Bautei­ len aus Titan oder Titanbasislegierungen bei 400-600°C getempert, jedoch werden anschließend die Nickeldeckschicht und die Diffusionsschicht TiNi3 che­ misch entfernt. Dadurch wird die Oberfläche aufgerauht, was eine mechanische Verankerung der folgenden Beschichtung ermöglichen soll. Diese Aufrauhung der Oberfläche hat sich als nachteilig erwiesen.In DE-OS 36 22 032 this is attempted with a nickel sulfamate electrolyte at 5 A / dm 2 and 55 ° C. for 10 minutes. However, it is not possible to deposit layers with sufficient adhesion from such electrolytes, since the residual stresses of the layers lie in the tensile stress range. In DE 33 21 231, electrolessly deposited nickel layers on surfaces of components made of titanium or titanium-based alloys are annealed at 400-600 ° C., however, the nickel cover layer and the diffusion layer TiNi 3 are then removed chemically. This will roughen the surface, which should allow the subsequent coating to be mechanically anchored. This roughening of the surface has proven to be disadvantageous.

Aufgabe der vorliegenden Erfindung ist die Schaffung eines Verfahrens der ein­ gangs bezeichneten Art, mit dem sich haftfeste Nickelschichten auf Titan oder Titanlegierungen ohne vorherige Aufrauhung der Oberfläche herstellen lassen.The object of the present invention is to create a method of a initially described type with which adherent nickel layers on titanium or Allow titanium alloys to be made without roughening the surface.

Diese Aufgabe wird erfindungsgemäß gelöst durch ein Verfahren gemäß dem kenn­ zeichnenden Teil des Patentanspruchs. This object is achieved according to the invention by a method according to the characteristic drawing part of the claim.  

Weitere Ausgestaltungen der Erfindung sind den Kennzeichnungsteilen der Unter­ ansprüche zu entnehmen.Further refinements of the invention are the labeling parts of the sub claims.

In dem erfindungsgemäßen Verfahren wird auf den Behandlungsschritt der Aufrau­ hung der Oberfläche vermieden, was nicht nur zu einer homogeneren Oberflächen­ struktur führt, sondern auch insgesamt eine einfachere Handhabung gewährlei­ stet. Weiterhin ist es bei dem erfindungsgemäßen Verfahren unabhängig, ob die Wärmebehandlung nach der außenstromlosen Abscheidung der Nickel-Phosphor-Le­ gierung oder erst nach der endgültigen dekorativen oder funktionellen Beschich­ tung erfolgt.In the method according to the invention, the roughening is carried out on the treatment step surface avoidance, which not only results in more homogeneous surfaces structure leads, but also overall easier handling continuous Furthermore, it is independent of the method according to the invention whether the Heat treatment after electroless plating of the nickel-phosphorus le alloy or only after the final decorative or functional coating tion takes place.

Die außenstromlose Abscheidung der Nickel-Phosphor-Erfindung erfolgt in an sich bekannter Weise unter Verwendung üblicher chemischer Nickelbäder.The electroless plating of the nickel-phosphor invention takes place in itself known manner using conventional chemical nickel baths.

Die folgenden Beispiele dienen zur Erläuterung der Erfindung mit den folgenden Verfahrensschritten:
The following examples serve to illustrate the invention with the following process steps:

Beispiel 1example 1

  • - Es wird Titan beschichtet.- Titanium is coated.
  • - Entfetten- degrease
  • - Spülen- Do the washing up
  • - Tauchen in 5%iger HF-Lösung, 5 Sekunden, 40°C- Diving in 5% HF solution, 5 seconds, 40 ° C
  • - Spülen- Do the washing up
  • - Vernickeln in einem außenstromlosen Nickelbad- Nickel plating in an electroless nickel bath
  • - Spülen- Do the washing up
  • - Vergolden in einem elektrolytischen Goldbad- Gold plating in an electrolytic gold bath
  • - Wärmebehandlung bei 600°C für eine Stunde- Heat treatment at 600 ° C for one hour
Beispiel 2Example 2

  • - Tauchen in 5%iger HF-Lösung, 5 Sekunden, 40°C- Diving in 5% HF solution, 5 seconds, 40 ° C
  • - Spülen- Do the washing up
  • - Vernickeln in einem außenstromlosen Nickelbad- Nickel plating in an electroless nickel bath
  • - Wärmebehandlung bei 650°C für 30 Minuten- Heat treatment at 650 ° C for 30 minutes
  • - Entfetten- degrease
  • - Spülen- Do the washing up
  • - Vergolden in einem elektrolytischen Goldbad- Gold plating in an electrolytic gold bath

Claims (5)

1. Verfahren zur haftfesten Metallisierung von Titan oder Titanlegierungen durch außenstromlose Abscheidung einer Nickel-Phosphor-Legierung mit an­ schließender Wärmebehandlung zur Ausbildung von Nickel-Titan-Diffusions­ schicht, dadurch gekennzeichnet, daß die danach noch vorhandene Nickel­ schicht haftfest metallisiert wird.1. A method for the adhesive metallization of titanium or titanium alloys by electroless deposition of a nickel-phosphorus alloy with subsequent heat treatment to form nickel-titanium diffusion layer, characterized in that the nickel which is still present thereafter is metallized in an adherent manner. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Titan oder die Titanlegierungen vor der außenstromlosen Abscheidung einer Nickel-Phosphor- Legierung in einer fluoridhaltigen Lösung gereinigt werden.2. The method according to claim 1, characterized in that the titanium or the Titanium alloys before electroless plating of a nickel-phosphorus Alloy can be cleaned in a fluoride-containing solution. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die fluoridhaltige Lösung Flußsäure oder Alkalifluorid in Konzentrationen von 0,01% bis zur Löslichkeitsgrenze enthält.3. The method according to claim 2, characterized in that the fluoride-containing Solution hydrofluoric acid or alkali fluoride in concentrations from 0.01% to Contains solubility limit. 4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß nach dem Beschichten eine Wärmebehandlung bei Temperaturen über 200°C durchgeführt wird.4. The method according to claim 1, characterized in that after the coating a heat treatment is carried out at temperatures above 200 ° C. 5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die Wärmebehandlung unter Schutzgas oder im Vakuum durchgeführt wird.5. The method according to claim 4, characterized in that the heat treatment is carried out under protective gas or in a vacuum.
DE19883816495 1988-05-10 1988-05-10 METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS Withdrawn DE3816495A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE19883816495 DE3816495A1 (en) 1988-05-10 1988-05-10 METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS
EP89107902A EP0341546A3 (en) 1988-05-10 1989-05-02 Process for depositing an adherent metal layer on titanium or its alloys
JP11524189A JPH0270073A (en) 1988-05-10 1989-05-10 Method for coating metal with for coating metal with titanium or titanium alloy in strongly bonded state

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19883816495 DE3816495A1 (en) 1988-05-10 1988-05-10 METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS

Publications (1)

Publication Number Publication Date
DE3816495A1 true DE3816495A1 (en) 1989-11-23

Family

ID=6354377

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19883816495 Withdrawn DE3816495A1 (en) 1988-05-10 1988-05-10 METHOD FOR ADHESIVE METALIZATION OF TITANIUM OR TITANIUM ALLOYS

Country Status (3)

Country Link
EP (1) EP0341546A3 (en)
JP (1) JPH0270073A (en)
DE (1) DE3816495A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU3553599A (en) * 1998-04-13 1999-11-01 Acm Research, Inc. Method and apparatus for enhancing adhesion between barrier layer and metal layer formed by plating

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62124290A (en) * 1985-11-22 1987-06-05 Citizen Watch Co Ltd Plate method to titanium surface

Also Published As

Publication number Publication date
JPH0270073A (en) 1990-03-08
EP0341546A2 (en) 1989-11-15
EP0341546A3 (en) 1990-05-16

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