EP0054743B1 - Procédé d'élimination chimique de couches d'oxyde sur des objets en titane ou alliage de titane - Google Patents

Procédé d'élimination chimique de couches d'oxyde sur des objets en titane ou alliage de titane Download PDF

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Publication number
EP0054743B1
EP0054743B1 EP81109537A EP81109537A EP0054743B1 EP 0054743 B1 EP0054743 B1 EP 0054743B1 EP 81109537 A EP81109537 A EP 81109537A EP 81109537 A EP81109537 A EP 81109537A EP 0054743 B1 EP0054743 B1 EP 0054743B1
Authority
EP
European Patent Office
Prior art keywords
titanium
fluoride
removal
alkali
oxide layer
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.)
Expired
Application number
EP81109537A
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German (de)
English (en)
Other versions
EP0054743A1 (fr
Inventor
Ludwig Fahrmbacher-Lutz
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Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Publication of EP0054743A1 publication Critical patent/EP0054743A1/fr
Application granted granted Critical
Publication of EP0054743B1 publication Critical patent/EP0054743B1/fr
Expired legal-status Critical Current

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Classifications

    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/106—Other heavy metals refractory metals
    • 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
    • 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
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C25F1/08—Refractory metals

Definitions

  • the invention relates to a method for the chemical removal of oxide layers from objects made of titanium or titanium alloys for subsequent coating with metals, in particular in an organic electrolyte.
  • the invention therefore has for its object to provide a method by means of which it is possible to effectively remove the oxide films from workpieces made of titanium or titanium alloys without impairing the dimensional accuracy of the workpieces and the material properties, for example of screws.
  • the organic media used are those in which both the hydrogen fluoride and alkali metal fluoride or ammonium fluoride can be dissolved.
  • the media preferably consist of alcohols, in particular methanol.
  • the treatment is preferably carried out with a medium containing 3 to 8% by weight of hydrogen fluoride, 5 to 8% by weight of ammonium fluoride and 5 to 10% by weight of an alkali fluoride, in particular sodium fluoride.
  • the treatment temperature is preferably between 10 ° C and 50 ° C.
  • the removal of the oxide layer can preferably be supported electrochemically by the process according to the invention, the procedure being in particular such that adding an alkali metal salt, for.
  • an alkali metal salt for.
  • the z. B. can consist of titanium or platinum, the workpieces alternately anodic and cathodic switches.
  • the workpieces are preferably rinsed with an inert solvent under a water vapor and oxygen-free atmosphere, in particular in an inert gas atmosphere, whereby they are fed to the device in which the metal coating, preferably by electrolytic means, is also carried out under oxygen and water vapor-free conditions , takes place, in particular as metals to be layered aluminum, copper, nickel and silver, but also germanium, beryllium, molybdenum, tungsten and Zirconium.
  • electrolytic deposition known electrolyte systems can be used (US Pat. No. 2,763,605; Hurley FH, Wier TP "Electrodeposition of AI from nonaquous solutions", J. Elektrochem. Soc.
  • a workpiece consisting of titanium is fastened to a suitable device, which ensures safe handling and safe electrical contact.
  • the part is then in methanol, which is also with z.
  • B. is oxygen and hydrogen-free argon saturated, free of grease residues and any other adhering particles.
  • the workpiece Under inert gas, the workpiece is placed in a pickling solution consisting of a methanolic solution of 8% hydrogen fluoride, 5% ammonium fluoride and 10% sodium fluoride.
  • This solution contains platinum electrodes which, like the workpiece, are connected to a voltage source. These make it possible to change the potential from +10 V to -10 V within one second.
  • a voltage ratio of anode / cathode 2-1 is maintained at a temperature of 15 ° C, with the current direction changing every 10 seconds. The process described is complete after about 3 minutes.
  • the electrolyte consists of an ethereal solution of 3 mol of aluminum chloride and approx. 1 mol of LiH or LiAIH 4 and allows smooth, reversing direct current at a current density of approx. 3 A / Dm 2 . to deposit dense aluminum layers of approx. 0.08 cm, whereby an excellent adhesion to the base material is achieved.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • ing And Chemical Polishing (AREA)
  • Physical Vapour Deposition (AREA)

Claims (8)

1. Procédé d'élimination chimique des couches d'oxyde sur des objets en titane ou alliages de titante en vue de les revôtir ensuite de métaux caractérisé par le fait que l'on effectue ce traitement dans une solution organique anhydre d'un mélange de fluorure d'hydrogène et d'un ou plusieurs fluorures alcalins et/ou de fluorure d'ammonium.
2. Procédé selon la revendication 1, caractérisé par le fait que la solution utilisée est formée d'un alcool anhydre avec une teneur de 3 à 8% en poids de fluorure d'hydrogène, de 5 à 8% en poids de fluorure d'ammonium et de 5 à 10% en poids d'un fluorure alcalin.
3. Procédé selon la revendication 2, caractérisé par le fait que l'alcool anhydre utilisé est formé de méthanol.
4. Procédé selon les revendications 1 à 3, caractérisé par le fait que le fluorure alcalin utilisé est formé de fluorure de sodium.
5. Procédé selon les revendications 1 à 4, caractérisé par le fait que l'on effecture le traitment à une température de 10 à 50° C.
6. Procédé selon les revendications 1 à 5, caractérisé par le fait que l'on assiste par voie électrochimique l'élimination de la couche d'oxyde.
7. Procédé selon la revendication 6, caractérisé par le fait que l'assistance électrochimique à l'élimination de la couche d'oxyde s'effectue par addition de sels alcalins pour l'augmentation de la conductivité de la solution et au moyen d'électrodes opposés.
8. Procédé selon les revendications 1 à 7, caractérisé par le fait que l'on rince les pièces débarrassées de la couche d'oxyde, avant de les revêtir d'un métal, avec un solvant inerte dans une atmosphère exempte de vapeur d'eau et d'oxygène.
EP81109537A 1980-12-19 1981-11-05 Procédé d'élimination chimique de couches d'oxyde sur des objets en titane ou alliage de titane Expired EP0054743B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3048083 1980-12-19
DE3048083A DE3048083C2 (de) 1980-12-19 1980-12-19 Verfahren zur chemischen Entfernung von Oxidschichten von Gegenständen aus Titan oder Titanlegierungen

Publications (2)

Publication Number Publication Date
EP0054743A1 EP0054743A1 (fr) 1982-06-30
EP0054743B1 true EP0054743B1 (fr) 1985-01-23

Family

ID=6119718

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81109537A Expired EP0054743B1 (fr) 1980-12-19 1981-11-05 Procédé d'élimination chimique de couches d'oxyde sur des objets en titane ou alliage de titane

Country Status (3)

Country Link
US (1) US4525250A (fr)
EP (1) EP0054743B1 (fr)
DE (1) DE3048083C2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0267534A1 (fr) * 1986-11-11 1988-05-18 INTERATOM Gesellschaft mit beschränkter Haftung Procédé et dispositif pour le dépôt galvanique de métaux sur un substrat
EP0504705A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0504704A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
DE19533748A1 (de) * 1995-09-12 1997-03-13 Alcotec Beschichtungsanlagen G Aktivierungslösung zur Aktivierung von metallischen Werkstoffen und Verfahren zur Aktivierung von metallischen Werkstoffen
DE10057560A1 (de) * 2000-11-21 2002-05-23 Volkswagen Ag Verfahren zur Erhöhung einer Korrosionsbeständigkeit eines Werkstücks aus Titan oder einer Titanlegierung und Verwendung des Verfahrens

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DE3344958C1 (de) * 1983-12-13 1984-07-19 VEGLA Vereinigte Glaswerke GmbH, 5100 Aachen Verfahren zum Verloeten eines Stromanschlusselementes mit dem Stromzufuehrungsleiter einer heizbaren Glasscheibe
US4968383A (en) * 1985-06-18 1990-11-06 The Dow Chemical Company Method for molding over a preform
US4861407A (en) * 1985-06-18 1989-08-29 The Dow Chemical Company Method for adhesive bonding articles via pretreatment with energy beams
US4755263A (en) * 1986-09-17 1988-07-05 M&T Chemicals Inc. Process of electroplating an adherent chromium electrodeposit on a chromium substrate
DE4120305C1 (fr) * 1991-06-20 1992-08-27 Mtu Muenchen Gmbh
AT403931B (de) * 1993-07-08 1998-06-25 Andritz Patentverwaltung Verfahren und vorrichtung zur nachbehandlung von gebeizten stahlprodukten, insbesondere von gebeiztem c-stahl-warmband
US5464524A (en) * 1993-09-17 1995-11-07 The Furukawa Electric Co., Ltd. Plating method for a nickel-titanium alloy member
US5376236A (en) * 1993-10-29 1994-12-27 At&T Corp. Process for etching titanium at a controllable rate
US6800326B1 (en) * 1997-01-14 2004-10-05 Seiko Epson Corporation Method of treating a surface of a surface of a substrate containing titanium for an ornament
US6416589B1 (en) 1999-02-18 2002-07-09 General Electric Company Carbon-enhanced fluoride ion cleaning
US6248704B1 (en) 1999-05-03 2001-06-19 Ekc Technology, Inc. Compositions for cleaning organic and plasma etched residues for semiconductors devices
US6537816B1 (en) * 1999-06-14 2003-03-25 General Electric Company Standards, methods for making, and methods for using the standards in evaluation of oxide removal
ES2159477B1 (es) * 1999-08-17 2002-04-16 Montana Exposito Vicenta De Procedimiento por el que un zapato infantil o deportivo se recubre de metal transformandose en objeto decorativo o trofeo.
US6355116B1 (en) 2000-03-24 2002-03-12 General Electric Company Method for renewing diffusion coatings on superalloy substrates
US6527938B2 (en) 2001-06-21 2003-03-04 Syntheon, Llc Method for microporous surface modification of implantable metallic medical articles
US6913791B2 (en) * 2003-03-03 2005-07-05 Com Dev Ltd. Method of surface treating titanium-containing metals followed by plating in the same electrolyte bath and parts made in accordance therewith
US6932897B2 (en) * 2003-03-03 2005-08-23 Com Dev Ltd. Titanium-containing metals with adherent coatings and methods for producing same
US6960370B2 (en) * 2003-03-27 2005-11-01 Scimed Life Systems, Inc. Methods of forming medical devices
US6878215B1 (en) 2004-05-27 2005-04-12 General Electric Company Chemical removal of a metal oxide coating from a superalloy article
US7611588B2 (en) * 2004-11-30 2009-11-03 Ecolab Inc. Methods and compositions for removing metal oxides
US7115171B2 (en) * 2004-12-27 2006-10-03 General Electric Company Method for removing engine deposits from turbine components and composition for use in same
DE102007043479A1 (de) * 2007-09-12 2009-03-19 Valeo Schalter Und Sensoren Gmbh Verfahren zur Oberflächenbehandlung von Aluminium und ein Schichtaufbau eines Bauteils aus Aluminium mit einer elektrischen Kontaktierung
EP2570520B1 (fr) * 2011-09-15 2017-11-22 General Electric Company Procédé de régénération d'une structure multicouche
CN102560514A (zh) * 2012-01-16 2012-07-11 南昌航空大学 一种用于退除钛及钛合金阳极氧化膜的弱酸性悬浮液
CN104947162A (zh) * 2015-07-22 2015-09-30 四川华丰企业集团有限公司 一种钛合金表面电镀方法

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GB922507A (en) * 1961-09-28 1963-04-03 Continental Titanium Metals Co Improvements in and relating to the conditioning of titanium or titanium base alloys
US3468774A (en) * 1966-12-09 1969-09-23 Rohr Corp Electrolytic descaling of titanium and its alloys
DE1621595A1 (de) * 1967-01-09 1971-04-29 Hilvolin Gmbh Verfahren zum Entfernen von Rost,Zunder,Walzhaut und kieselsaeurehaltigen Belaegen von Eisen- und Stahloberflaechen mittels einer Beizfluessigkeit
US3562013A (en) * 1967-10-23 1971-02-09 Diversey Corp Process of deoxidizing titanium and its alloys
DE1621177B2 (de) * 1967-12-08 1976-09-30 Siemens AG, 1000 Berlin und 8000 München Verfahren zur galvanischen herstellung von nickel-, kupfer-, zink-, indium-, zinn- und goldueberzuegen auf niob und niob-zirkon-legierungen
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DD149086A1 (de) * 1979-07-04 1981-06-24 Hans H Daut Verfahren zur minimierung des uebergangswiderstandes von aluminium in elektrischen verbindungen
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0267534A1 (fr) * 1986-11-11 1988-05-18 INTERATOM Gesellschaft mit beschränkter Haftung Procédé et dispositif pour le dépôt galvanique de métaux sur un substrat
NL8602856A (nl) * 1986-11-11 1988-06-01 Hga Galvano Aluminium B V Werkwijze en inrichting voor het galvanisch afscheiden van metalen op een substraat.
EP0504705A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
EP0504704A1 (fr) * 1991-03-20 1992-09-23 Siemens Aktiengesellschaft Prétraitement pour matériaux métalliques pour la déposition de métaux par électrolyse
DE19533748A1 (de) * 1995-09-12 1997-03-13 Alcotec Beschichtungsanlagen G Aktivierungslösung zur Aktivierung von metallischen Werkstoffen und Verfahren zur Aktivierung von metallischen Werkstoffen
DE19533748C2 (de) * 1995-09-12 2000-09-14 Rasant Alcotec Beschichtungste Aktivierungslösung zur Vorbehandlung von metallischen Werkstoffen für die galvanische Metallbeschichtung aus nicht wäßrigen Elektrolyten, Verwendung und Verfahren
DE10057560A1 (de) * 2000-11-21 2002-05-23 Volkswagen Ag Verfahren zur Erhöhung einer Korrosionsbeständigkeit eines Werkstücks aus Titan oder einer Titanlegierung und Verwendung des Verfahrens

Also Published As

Publication number Publication date
DE3048083C2 (de) 1983-09-29
EP0054743A1 (fr) 1982-06-30
US4525250A (en) 1985-06-25
DE3048083A1 (de) 1982-07-01

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