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EP1713955A1 - Passivation noire de surfaces en zinc ou alliage de zinc - Google Patents

Passivation noire de surfaces en zinc ou alliage de zinc

Info

Publication number
EP1713955A1
EP1713955A1 EP05700867A EP05700867A EP1713955A1 EP 1713955 A1 EP1713955 A1 EP 1713955A1 EP 05700867 A EP05700867 A EP 05700867A EP 05700867 A EP05700867 A EP 05700867A EP 1713955 A1 EP1713955 A1 EP 1713955A1
Authority
EP
European Patent Office
Prior art keywords
solution
solution according
passivation
chromium
zinc
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
Application number
EP05700867A
Other languages
German (de)
English (en)
Other versions
EP1713955B1 (fr
Inventor
Bertram Haag
Peter Herold
Rainer Dillinger
Sergej Vogelsang
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.)
Schaeffler Technologies AG and Co KG
Original Assignee
Schaeffler KG
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 Schaeffler KG filed Critical Schaeffler KG
Publication of EP1713955A1 publication Critical patent/EP1713955A1/fr
Application granted granted Critical
Publication of EP1713955B1 publication Critical patent/EP1713955B1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/53—Treatment of zinc or alloys based thereon
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/84—Dyeing
    • 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
    • C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium

Definitions

  • the invention relates to an aqueous solution for improving the black passivation of zinc or zinc alloy surfaces.
  • the invention also relates to associated methods for black passivation.
  • Metallic materials are galvanized to protect them from corrosive environmental influences.
  • the protection against corrosion of the zinc is based on the fact that it is even less noble than the base metal and therefore initially only attracts the corrosive attack, it acts as a sacrificial layer.
  • the base metal of the galvanized component in question remains intact as long as it is continuously covered with zinc and the mechanical functionality is retained over longer periods than with non-galvanized parts. Thick layers of zinc provide greater protection against corrosion than thin layers because the corrosive removal of thick layers takes longer.
  • the corrosive attack on the zinc layer in turn, can be greatly delayed by the application of chromate, and thus the base metal corrosion is also delayed further than by galvanizing alone.
  • the corrosion protection provided by the zinc / chromating layer system is considerably higher than that of a zinc layer of the same thickness. Chromating also delays the visual impairment of a component due to environmental influences, and the corrosion products of zinc, the so-called white rust, also have a disruptive effect on the appearance of a component.
  • the advantage The chromate applied is so large that almost every galvanized surface is also chromated.
  • the corrosion protection of undamaged black chromations based on chromium (VI) amounts to 50-150 hours in the salt spray test according to DIN 50021 SS. This corrosion test exposes a coated and passivated part to a 5% sodium chloride mist at 35 ° C and 100% humidity , The time required to oxidize 5 - 10% of the surface to white rust is measured.
  • the trivalent chromium is formed from hexavalent chromium by the addition of a reducing agent such as an aldehyde or alcohol, an alkali metal sulfite, bisulfite, iodide, hydrogen peroxide, sulfur dioxide or an iron salt. Since the conversion to chromium (IM) is not complete, it is possible that chromium (VI) in the passivation layer it is possible for chromium (VI) to be incorporated into the passivation layer, which is not particularly desirable when using such coatings in the food industry.
  • a reducing agent such as an aldehyde or alcohol, an alkali metal sulfite, bisulfite, iodide, hydrogen peroxide, sulfur dioxide or an iron salt.
  • EP 0 479 289 A1 describes a process in which phosphoric acid and hydrofluoric acid are present in the solution in a specific ratio to the chromium (III) ions and lead to a passivation surface of improved resistance.
  • Passivations based on chrome (Ill) are therefore used in two ways.
  • thin-film passivation with an additional post-treatment by sealing which is also referred to as a top coat.
  • This is to be understood as aftertreatment with wax-based, silicate or polymer-based agents.
  • thick film passivation which work with higher chromium concentrations and special stabilizers at higher temperatures and require longer exposure times.
  • Such layers have the thicknesses of common yellow or olive chromate layers and can be applied without sealing.
  • black chromating which is of particular importance for zinc alloys, there are particular problems since, although these can be carried out using known solutions for other chromating processes, they offer unsatisfactory corrosion protection. This can only be improved by a top coat coating.
  • top-coat covers cannot be rolled over and cannot be used for press and joint seats.
  • the object of the invention is therefore to provide an aqueous solution for the treatment of zinc or zinc alloy surfaces which, in the case of black passivation, enables substantially improved results in the formation of a chromium (VI) -free, homogeneous protective film of high corrosion resistance.
  • this object is achieved according to the characterizing part of claim 1 in that the solution contains inorganic and / or organic sulfur compounds.
  • the corrosion protection effect of protective layers consisting of chromium (III) ions can be significantly increased by the addition according to the invention. That's because to be attributed to the fact that the iron-sulfur pigments according to the invention which produce the black color improve the anti-corrosion effect of the protective layer, while the iron-phosphor pigments according to the prior art impair the anti-corrosion effect.
  • the inorganic and / or organic sulfur compounds can be handled in different ways. On the one hand, the aqueous solution with the sulfur compounds can be prepared as a separate solution and used immediately before or after the actual passivation of the surfaces, this being possible, for example, by a simple immersion process. On the other hand, it is also possible that the sulfur compounds according to the invention are added to the passivation solution used and in this way significantly improve the corrosion protection.
  • the associated different methods are described in claims 12, 13 and 14.
  • the solution contains salts or anhydrides of the following acids:
  • Hydrogen sulfide H 2 S
  • Thiosulfuric acid H 2 S 2 0 3
  • Disulphurous acid H 2 S 2 0 5
  • the solution should contain sulfur compounds in the form of alkali sulfite and / or alkali disulfite, especially sodium sulfite and / or sodium disulfite.
  • the dosage is evident from claims 6, 7 and 8. It is provided according to claim 6 that the solution contains 2-10 g / l, preferably 5 g / l sodium sulfite. According to claim 7, the solution should contain 2-10 g / l, preferably 6 g / l sodium disulfite. It is apparent from claim 8 that the solution should contain 2-10 g / l sodium sulfite and sodium disulfite, the two agents being usable in any mixing ratio.
  • the solution and thus the inorganic and / or organic sulfur compounds should be added to known passivation solutions, be free of chromium (VI) ions, contain chromium (III) ions and work in the acidic range.
  • Such a passivation solution known per se is derived from claim 10. Thereafter, it should contain chromium (III) ions acid and fluoride ions.
  • Such a solution could have the following composition, for example:
  • a steel component for a valve train of an internal combustion engine is provided with a corrosion protection layer made of a ZnFe alloy.
  • the electroplated layer has an alloying content of Fe of 0.8% and a layer thickness of 8 ⁇ m.
  • the steel component coated in this way was exposed to a chromium (III) -containing passivation solution from COVENTYA GmbH, which is sold under the trade name LANTHANE 315. This includes in accordance with the safety data among others chromium - (HO- nitrate and cobalt nitrate hexahydrate After setting a p H -value in the range of 1, 8 -.
  • the solution is ready for use, wherein the operating temperature is in the range from 40 to 70 °, preferably at 60 ° C. 5 g / l sodium sulfite were added to this passivation solution prepared in this way.
  • the steel component was immersed in the passivation solution for about 60 seconds and then rinsed several times in running water and finally dried.
  • the applied passivation layer showed a deep black color and was free of Cr (VI), as a corresponding test showed.
  • the passivated steel component was then subjected to the corrosion test according to DIN 50021 SS, the corrosion protection effect being many times higher than that of commercially available black passivation layers.
  • the corrosion protection performance achieved was> 1400 h.

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

L'invention concerne une solution aqueuse servant à améliorer la passivation noire de surfaces en zinc ou alliage de zinc. Cette solution est caractérisée en ce qu'elle contient des composés de soufre inorganique et/ou organique, ce qui permet d'obtenir une amélioration considérable de la protection contre la corrosion.
EP05700867.4A 2004-01-14 2005-01-13 Passivation noire de surfaces en zinc ou alliage de zinc Ceased EP1713955B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200410001945 DE102004001945A1 (de) 2004-01-14 2004-01-14 Schwarzpassivierung von Zink- oder Zinklegierungsoberflächen
PCT/EP2005/000250 WO2005068684A1 (fr) 2004-01-14 2005-01-13 Passivation noire de surfaces en zinc ou alliage de zinc

Publications (2)

Publication Number Publication Date
EP1713955A1 true EP1713955A1 (fr) 2006-10-25
EP1713955B1 EP1713955B1 (fr) 2013-06-19

Family

ID=34744715

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05700867.4A Ceased EP1713955B1 (fr) 2004-01-14 2005-01-13 Passivation noire de surfaces en zinc ou alliage de zinc

Country Status (3)

Country Link
EP (1) EP1713955B1 (fr)
DE (1) DE102004001945A1 (fr)
WO (1) WO2005068684A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007060185A1 (de) * 2007-12-14 2009-06-18 Siemens Ag Verfahren zum Beschichten einer metallischen Oberfläche sowie Beschichtungssystem
DE102009045569A1 (de) 2009-10-12 2011-04-14 Dr.-Ing. Max Schlötter GmbH & Co KG Schwarzpassivierung von Zink- und Zinkeisenschichten
EP3428314B1 (fr) 2017-07-14 2019-11-13 Ewald Dörken Ag Composition et procédé de passivation de composants galvanisés

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2302643A (en) * 1941-05-26 1942-11-17 Parker Rust Proof Co Method and composition for treating metals
US2902394A (en) * 1956-07-19 1959-09-01 Poor & Co Protective metal coating compositions and method of coating
US4171231A (en) * 1978-04-27 1979-10-16 R. O. Hull & Company, Inc. Coating solutions of trivalent chromium for coating zinc surfaces
US4263059A (en) * 1979-12-21 1981-04-21 Rohco, Inc. Coating solutions of trivalent chromium for coating zinc and cadmium surfaces
JPS6431982A (en) * 1987-07-29 1989-02-02 Nippon Steel Corp Black plated steel sheet and its production
US4968391A (en) * 1988-01-29 1990-11-06 Nippon Steel Corporation Process for the preparation of a black surface-treated steel sheet
DE20121187U1 (de) * 2001-12-20 2002-06-13 Walter Hillebrand GmbH & Co., 58739 Wickede Schwarzpassivierungsgemisch
DE10162756A1 (de) * 2001-12-20 2003-07-10 Walter Hillebrand Gmbh & Co Schwarzpassivierungsverfahren
JP4312985B2 (ja) * 2002-01-22 2009-08-12 日本表面化学株式会社 金属表面の黒色皮膜形成処理方法
JP3774415B2 (ja) * 2002-03-14 2006-05-17 ディップソール株式会社 亜鉛及び亜鉛合金めっき上に黒色の六価クロムフリー化成皮膜を形成するための処理溶液及び亜鉛及び亜鉛合金めっき上に黒色の六価クロムフリー化成皮膜を形成する方法。
US20040156999A1 (en) * 2003-02-07 2004-08-12 Pavco, Inc. Black trivalent chromium chromate conversion coating
DE10305450A1 (de) * 2003-02-11 2004-08-26 Walter Hillebrand Gmbh & Co. Aktivatoren der Schwarzpassivierung

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2005068684A1 *

Also Published As

Publication number Publication date
WO2005068684A1 (fr) 2005-07-28
DE102004001945A1 (de) 2005-08-11
EP1713955B1 (fr) 2013-06-19

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