EP0072986A1 - Procédé pour l'activation des surfaces de titane - Google Patents
Procédé pour l'activation des surfaces de titane Download PDFInfo
- Publication number
- EP0072986A1 EP0072986A1 EP82107356A EP82107356A EP0072986A1 EP 0072986 A1 EP0072986 A1 EP 0072986A1 EP 82107356 A EP82107356 A EP 82107356A EP 82107356 A EP82107356 A EP 82107356A EP 0072986 A1 EP0072986 A1 EP 0072986A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- acid
- solution
- activation
- activating
- hexafluorosilicic
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000010936 titanium Substances 0.000 title claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 7
- 230000004913 activation Effects 0.000 title claims description 14
- 230000008569 process Effects 0.000 title claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003213 activating effect Effects 0.000 claims abstract description 8
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims abstract description 5
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims abstract 2
- -1 hexafluorosilicic acid Chemical compound 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000005422 blasting Methods 0.000 abstract description 4
- 238000005253 cladding Methods 0.000 abstract 1
- 238000005530 etching Methods 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910003638 H2SiF6 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WIUHYQBOXHNHLG-UHFFFAOYSA-N acetic acid hydrofluoride Chemical compound F.C(C)(=O)O WIUHYQBOXHNHLG-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 150000001463 antimony compounds Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940093920 gynecological arsenic compound Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229960002050 hydrofluoric acid Drugs 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- ZEFWRWWINDLIIV-UHFFFAOYSA-N tetrafluorosilane;dihydrofluoride Chemical compound F.F.F[Si](F)(F)F ZEFWRWWINDLIIV-UHFFFAOYSA-N 0.000 description 1
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 subsequent plating with metallic coatings, in the course of which the surface is first wet-blasted with fine-grained A1 2 0 3 and then treated with a fluoride-containing solution for a few minutes at room temperature.
- German patent application P 30 08 314.8-45 a generic method has been proposed in which the surface is activated by wet blasting and pickling with a solution of chromic acid, hydrofluoric acid and arsenic or antimony compounds at temperatures of from 35 to 100 ° C and for a period of 15 to 50 minutes.
- This proposed method gives excellent adhesive properties in the subsequent plating with metallic top coats.
- arsenic and antimony solution however, the risk of side reactions cannot be completely ruled out, which then change the bath in such a way that the desired 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.
- the activation of the titanium surface takes place in such a way that the roughness of the surface is increased.
- a further advantage of the method according to the invention is that after activation (roughening of the surface) the titanium component can also be stored untreated for a long time, since the newly formed oxide skin is harmless for further treatment due to the adhesion process due to the enlarged surface.
- 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)
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 true EP0072986A1 (fr) | 1983-03-02 |
| EP0072986B1 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0120340A1 (fr) * | 1983-03-16 | 1984-10-03 | Mtu Motoren- Und Turbinen-Union MàNchen Gmbh | Procédé pour détecter des inhomogénéités de texture dans des échantillons et des pièces soudées en titane |
| EP0179013A1 (fr) * | 1984-10-16 | 1986-04-23 | United Technologies Corporation | Usinage chimique utilisant une particule inerte et un container mobile |
| US8354036B2 (en) | 2005-11-21 | 2013-01-15 | Mtu Aero Engines Gmbh | Method for the pre-treatment of titanium components for the subsequent coating thereof |
| WO2018015009A1 (fr) * | 2016-07-18 | 2018-01-25 | Ceramtec Gmh | Dépôt électrolytique de cuivre sur des métallisations réfractaires |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| US7611588B2 (en) * | 2004-11-30 | 2009-11-03 | Ecolab Inc. | Methods and compositions for removing metal oxides |
| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2229897A1 (de) * | 1971-06-17 | 1972-12-21 | Rolls Royce | Verfahren zum Atzen von aus Titan oder Titanlegierungen bestehenden Teilen |
| DE2315081A1 (de) * | 1972-03-31 | 1974-04-11 | Ppg Industries Inc | Verfahren zum behandeln von titangegenstaenden |
| US3891456A (en) * | 1973-10-17 | 1975-06-24 | Us Air Force | Surface treatment of titanium and titanium alloys |
| DE3008314A1 (de) * | 1980-03-04 | 1981-09-10 | MTU Motoren- und Turbinen-Union München GmbH, 8000 München | Verfahren zur aktivierung von titanoberflaechen |
Family Cites Families (4)
| 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 |
-
1981
- 1981-08-21 DE DE3133189A patent/DE3133189C2/de not_active Expired
- 1981-11-18 US US06/322,585 patent/US4414039A/en not_active Expired - Lifetime
-
1982
- 1982-08-13 DE DE8282107356T patent/DE3261695D1/de not_active Expired
- 1982-08-13 EP EP82107356A patent/EP0072986B1/fr not_active Expired
- 1982-08-13 AT AT82107356T patent/ATE10954T1/de not_active IP Right Cessation
- 1982-08-19 JP JP57143971A patent/JPS5842790A/ja active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2229897A1 (de) * | 1971-06-17 | 1972-12-21 | Rolls Royce | Verfahren zum Atzen von aus Titan oder Titanlegierungen bestehenden Teilen |
| DE2315081A1 (de) * | 1972-03-31 | 1974-04-11 | Ppg Industries Inc | Verfahren zum behandeln von titangegenstaenden |
| US3891456A (en) * | 1973-10-17 | 1975-06-24 | Us Air Force | Surface treatment of titanium and titanium alloys |
| DE3008314A1 (de) * | 1980-03-04 | 1981-09-10 | MTU Motoren- und Turbinen-Union München GmbH, 8000 München | Verfahren zur aktivierung von titanoberflaechen |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0120340A1 (fr) * | 1983-03-16 | 1984-10-03 | Mtu Motoren- Und Turbinen-Union MàNchen Gmbh | Procédé pour détecter des inhomogénéités de texture dans des échantillons et des pièces soudées en titane |
| EP0179013A1 (fr) * | 1984-10-16 | 1986-04-23 | United Technologies Corporation | Usinage chimique utilisant une particule inerte et un container mobile |
| US8354036B2 (en) | 2005-11-21 | 2013-01-15 | Mtu Aero Engines Gmbh | Method for the pre-treatment of titanium components for the subsequent coating thereof |
| WO2018015009A1 (fr) * | 2016-07-18 | 2018-01-25 | Ceramtec Gmh | Dépôt électrolytique de cuivre sur des métallisations réfractaires |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0072986B1 (fr) | 1984-12-27 |
| 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 |
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