EP0072986B1 - Procédé pour l'activation des surfaces de titane - Google Patents

Procédé pour l'activation des surfaces de titane Download PDF

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Publication number
EP0072986B1
EP0072986B1 EP82107356A EP82107356A EP0072986B1 EP 0072986 B1 EP0072986 B1 EP 0072986B1 EP 82107356 A EP82107356 A EP 82107356A EP 82107356 A EP82107356 A EP 82107356A EP 0072986 B1 EP0072986 B1 EP 0072986B1
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EP
European Patent Office
Prior art keywords
acid
activation
solution
hexahydrofluorsilicic
activating
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.)
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Application number
EP82107356A
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German (de)
English (en)
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EP0072986A1 (fr
Inventor
Martin Dr.Rer.Nat. Thoma
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.)
MTU Aero Engines AG
Original Assignee
MTU Motoren und Turbinen Union Muenchen GmbH
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Application filed by MTU Motoren und Turbinen Union Muenchen GmbH filed Critical MTU Motoren und Turbinen Union Muenchen GmbH
Priority to AT82107356T priority Critical patent/ATE10954T1/de
Publication of EP0072986A1 publication Critical patent/EP0072986A1/fr
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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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/26—Acidic compositions for etching refractory metals

Definitions

  • the invention relates to a method for activating titanium surfaces for the subsequent plating with metallic coatings, in the course of which the surface is first wet-blasted with fine-grained Al 2 O 3 and then treated with a fluoride-containing solution for a few minutes at room temperature.
  • EP-A No. 0035241 (corresponding to DE-A1 No. 3008314), in which wet blasting and pickling involve activation of the surface with a solution of chromic acid, hydrofluoric acid and arsenic or antimony compounds at temperatures from 35 to 100 ° C and for a period of 15 to 50 min.
  • This proposed method gives excellent adhesive properties in the subsequent plating with metallic coatings.
  • arsenic and antimony solution however, the risk of side reactions cannot be completely ruled out, which then change the bath so that the intended activation function is not guaranteed. This makes it difficult to control and control the bathroom.
  • the object of the present invention is to improve a generic method in such a way that the activation bath can be precisely controlled and that it can be supplemented without difficulty, in particular after a long service life.
  • this object is achieved in that the wet blasting and pickling is followed by activation of the surface with a solution of chromic acid, hydrofluoric acid and hexafluorosilicic acid at temperatures of 35 to 100 ° C. and for a period of 15 to 50 minutes.
  • a particularly sustainable activation can be achieved if the components for activating the surface contain hexafluorosilicic acid, hydrofluoric acid and chromic acid in the following molar ratios (based on the elements):
  • the concentration of the hexafluorosilicic acid in the activation solution is less important for the achievable results, the hexafluorosilicic acid concentration should advantageously be chosen between 0.1 and 2.0 mol / l. Further advantageous refinements of this method are specified in subclaims 4 to 6.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemically Coating (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Coating With Molten Metal (AREA)
  • ing And Chemical Polishing (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
  • Catalysts (AREA)
  • Chemical Treatment Of Metals (AREA)

Claims (6)

1. Procédé pour l'activation des surfaces de titane en vue du placage ultérieur avec des revêtements métalliques, procédé dans lequel la surface est tout d'abord soumise à un sablage humide avec Al2O3 à grains fins et ensuite traitée pendant une durée d'un petit nombre de minutes à la température du local avec une solution contenant un fluorure, procédé caractérisé en ce que, à ce traitement, se raccorde une activation de la surface avec une solution d'acide chromique, d'acide fluorhydrique et d'acide hexafluosilicique à des températures de 35 à 100° C, pendant une durée de 15 à 50 min.
2. Procédé selon la revendication 1, caractérisé en ce que la solution pour l'activation de la surface comporte les parties constituantes d'acide hexafluosilicique, acide fluorhydrique et acide chromique, selon les rapports moléculaires suivants des éléments:
Figure imgb0008
Figure imgb0009
3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que la solution pour l'activation de la surface a une concentration en acide hexafluosilicique de 0,1 < H2SiF6≦ 2,0 mol/I.
4. Procédé selon les revendications 1 à 3, caractérisé en ce que, pour l'acide hexafluosilicique de la solution d'activation, du silicium est utilisé sous forme de combinaisons d'oxydes, d'acides, de fluorures ou de complexes fluorés.
5. Procédé selon les revendications 1 à 4, caractérisé en ce que le produit de décapage contenant un fluorure est, comme cela est en soi connu, une solution acide nitrique/acide fluorhydrique.
6. Procédé selon la revendication 5, caractérisé en ce que la concentration du produit de décapage, comme cela est en soi connu, est de: 400 g/I HN03 et 5 g/I HF.
EP82107356A 1981-08-21 1982-08-13 Procédé pour l'activation des surfaces de titane Expired EP0072986B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82107356T ATE10954T1 (de) 1981-08-21 1982-08-13 Verfahren zur aktivierung von titanoberflaechen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3133189A DE3133189C2 (de) 1981-08-21 1981-08-21 "Verfahren zur Aktivierung von Titanoberflächen"
DE3133189 1981-08-21

Publications (2)

Publication Number Publication Date
EP0072986A1 EP0072986A1 (fr) 1983-03-02
EP0072986B1 true EP0072986B1 (fr) 1984-12-27

Family

ID=6139848

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82107356A Expired EP0072986B1 (fr) 1981-08-21 1982-08-13 Procédé pour l'activation des surfaces de titane

Country Status (5)

Country Link
US (1) US4414039A (fr)
EP (1) EP0072986B1 (fr)
JP (1) JPS5842790A (fr)
AT (1) ATE10954T1 (fr)
DE (2) DE3133189C2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7611588B2 (en) 2004-11-30 2009-11-03 Ecolab Inc. Methods and compositions for removing metal oxides

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3309448C2 (de) * 1983-03-16 1985-06-05 MTU Motoren- und Turbinen-Union München GmbH, 8000 München Verfahren zum Erkennen von Gefügeinhomogenitäten in Titanlegierungsproben und Schweißlingen
DE3321231C2 (de) * 1983-06-11 1985-10-31 MTU Motoren- und Turbinen-Union München GmbH, 8000 München Verfahren zur Herstellung von Verschleißschutzschichten auf Oberflächen von Bauteilen aus Titan oder Titanbasislegierungen
US4563239A (en) * 1984-10-16 1986-01-07 United Technologies Corporation Chemical milling using an inert particulate and moving vessel
US5258098A (en) * 1991-06-17 1993-11-02 Cycam, Inc. Method of production of a surface adapted to promote adhesion
DE4224316C1 (en) * 1992-07-23 1993-07-29 Freiberger Ne-Metall Gmbh, O-9200 Freiberg, De Metal coating of titanium@ (alloys) - by oxidising in acidic, fluorine-free soln., removing oxide layer, treating with ultrasound, and galvanically coating
EP1104693B1 (fr) * 1999-04-08 2009-07-15 Showa Co., Ltd. Materiau composite au titane
TW511180B (en) * 2000-07-31 2002-11-21 Mitsubishi Chem Corp Mixed acid solution in etching process, process for producing the same, etching process using the same and process for producing semiconductor device
CA2430041A1 (fr) * 2003-05-26 2004-11-26 Eugene I. Moody Chaudiere a liquide atomise
DE102005055303A1 (de) * 2005-11-21 2007-05-24 Mtu Aero Engines Gmbh Verfahren zur Vorbehandlung von Titanbauteilen zur nachfolgenden Beschichtung derselben
JP5836985B2 (ja) * 2013-02-20 2015-12-24 三菱電機株式会社 金属めっきされたＴｉ材の製造方法および多孔質電極の製造方法
CN104005059A (zh) * 2014-06-11 2014-08-27 沈阳飞机工业（集团）有限公司 一种在tc1、tc2钛合金上电镀铬的方法
US10687956B2 (en) 2014-06-17 2020-06-23 Titan Spine, Inc. Corpectomy implants with roughened bioactive lateral surfaces
TWI726940B (zh) 2015-11-20 2021-05-11 美商泰坦脊柱股份有限公司 積層製造整形外科植入物之方法
WO2018015009A1 (fr) * 2016-07-18 2018-01-25 Ceramtec Gmh Dépôt électrolytique de cuivre sur des métallisations réfractaires
CN109688979A (zh) 2016-08-03 2019-04-26 泰坦脊椎公司 增强骨诱导的植入物表面
CN109338429B (zh) * 2018-11-12 2020-12-29 中国航发北京航空材料研究院 一种钛合金电镀铝前处理方法
CN116695121A (zh) * 2023-08-08 2023-09-05 德州正瑞健康科技有限公司 一种纯钛牙种植体的处理方法与装置

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2276353A (en) * 1935-09-28 1942-03-17 Parker Rust Proof Co Process of coating
US2946728A (en) * 1955-06-23 1960-07-26 Cleveland Pneumatic Ind Inc Adherent electroplating on titanium
US2829091A (en) * 1956-06-04 1958-04-01 Menasco Mfg Company Method for electroplating titanium
CA960119A (en) * 1971-12-09 1974-12-31 George F. Otto Prepaint treatment for zinciferous surfaces
US3891456A (en) * 1973-10-17 1975-06-24 Us Air Force Surface treatment of titanium and titanium alloys
DE3008314C2 (de) * 1980-03-04 1982-09-16 MTU Motoren- und Turbinen-Union München GmbH, 8000 München Verfahren zur Aktivierung von Titanoberflächen

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7611588B2 (en) 2004-11-30 2009-11-03 Ecolab Inc. Methods and compositions for removing metal oxides

Also Published As

Publication number Publication date
JPH0153360B2 (fr) 1989-11-14
DE3133189C2 (de) 1984-02-09
DE3133189A1 (de) 1983-03-17
JPS5842790A (ja) 1983-03-12
DE3261695D1 (en) 1985-02-07
ATE10954T1 (de) 1985-01-15
US4414039A (en) 1983-11-08
EP0072986A1 (fr) 1983-03-02

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