EP2319957B1 - Passivation noire de zinc et couches de fer et de zinc - Google Patents

Passivation noire de zinc et couches de fer et de zinc Download PDF

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Publication number
EP2319957B1
EP2319957B1 EP10175959.5A EP10175959A EP2319957B1 EP 2319957 B1 EP2319957 B1 EP 2319957B1 EP 10175959 A EP10175959 A EP 10175959A EP 2319957 B1 EP2319957 B1 EP 2319957B1
Authority
EP
European Patent Office
Prior art keywords
zinc
solution
passivation
ions
layers
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.)
Active
Application number
EP10175959.5A
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German (de)
English (en)
Other versions
EP2319957A1 (fr
Inventor
Dr. Manfred Jordan
Dr. Roland Pfiz
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.)
Dr Ing Max Schloetter GmbH and Co KG
Original Assignee
Dr Ing Max Schloetter GmbH and Co 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 Dr Ing Max Schloetter GmbH and Co KG filed Critical Dr Ing Max Schloetter GmbH and Co KG
Priority to SI201031381A priority Critical patent/SI2319957T1/sl
Publication of EP2319957A1 publication Critical patent/EP2319957A1/fr
Application granted granted Critical
Publication of EP2319957B1 publication Critical patent/EP2319957B1/fr
Active 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
    • 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
    • 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
    • C25D5/48—After-treatment of electroplated surfaces
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc

Definitions

  • the invention relates to an acidic, aqueous reaction solution for producing a black passivation layer on zinc and zinc iron layers, to a method in which this reaction solution is used, and to the black passivation layer obtainable by this method.
  • the galvanic coating of components made of iron or steel with zinc or zinc alloys is carried out on a large scale and has a high economic importance.
  • the deposited layers protect the base material against corrosion and thus lead to a high increase in the value of the components.
  • the corrosion protection of iron or steel by zinc or zinc alloys is based on the anodic protection mechanism. Zinc or zinc alloys are less electrochemical than the base material. The corrosion attack therefore begins on the coating and the base material remains protected against corrosion as long as a closed zinc or zinc alloy surface is present.
  • the applied less noble zinc or Zinc alloy coatings are therefore also known as Called "sacrificial layers".
  • a zinc nickel layer with> 16% nickel is the nobler component compared to iron or steel and therefore can no longer provide anodic corrosion protection. The deposition of such a layer on iron or steel would therefore lead to preferred base material corrosion inhomogeneities of the coating (pitting corrosion).
  • the color of the chromating layers can be varied by composition of the solutions and by the working parameters in the treatment. You can create blue, yellow or olive colored surfaces. In this order, the layer thickness of the conversion layers and thus the corrosion protection increases.
  • black chromating layers Furthermore, it is also possible to produce black chromating layers.
  • the black chromations for pure zinc coatings were often added silver salts in very low concentrations. By reaction with the zinc surface, the Silver ions reduced to metallic silver. This resulting in very finely divided form silver is incorporated into the forming chromate layer and acts there as a black pigment.
  • Black chromations can produce deep black, uniform surfaces that can be used for decorative purposes.
  • the incorporation of small amounts of silver in the layer can have a detrimental effect on the corrosion protection, since silver is a very noble metal and therefore corrosion can lead to local element formation and thereby deterioration of the corrosion protection.
  • the alloying partners iron, cobalt or nickel can be converted into their oxides by suitable composition of the chromating solutions. These then act as black pigments in the chromating layer. Addition of silver salts to produce black pigments is not required in these cases.
  • the problem of the decomposition of these sulfur compounds also remains, if one does not use the free acids, but their salts.
  • the acids underlying the salts are weaker acids than e.g. Nitric acid or sulfuric acid used to adjust the pH of passivation solutions. The dissociation of the corresponding salts is thereby shifted to the side of the free acids, which then in turn uses the decomposition of the compounds.
  • WO 2005/068684 A1 The formation of the black passivation layer leads to the formation of iron-sulfur pigments. Although the method should also be suitable for the black passivation of pure zinc coatings, this hardly seems possible because they contain no iron and thus no iron-sulfur pigments can be formed.
  • a black corrosion resistant coating on zinc alloys and a method for its production is disclosed in US Pat EP 1 409 157 B1 described.
  • the layers are generated in a two-step process. First, a passivation layer is formed in a passivation solution based on trivalent chromium compounds. This layer does not have a black appearance yet. In a second process step is then in a sealing solution, the Contains black pigments, submerged. Although it is possible to achieve layers with the desired black appearance, such a two-step process is undesirable in practice. The application of a seal based on organic compounds is not permitted in all applications. It is therefore more advantageous if the black optic can already be achieved by the passivation layer and not only by the additional step of sealing.
  • EP 1 484 432 A1 claims a treatment solution and method for depositing black passivation layers on zinc or zinc alloy layers.
  • a disadvantage of this method is the relatively complicated composition of the treatment solution.
  • the deposition of black passivation layers requires a very close ratio of nitrate to chromium.
  • the ratio NO - 3 / Cr 3+ should be less than 0.5 / 1.
  • the chromium concentration is preferably 0.5 to 10 g / l, corresponding to 0.001 to 0.19 mol / l. This results in a resulting nitrate concentration of not more than 0.0005 to 0.095 mol / l or 0.03 to 5.9 g / l.
  • the analysis of such low nitrate concentrations is very difficult with the analytical methods that are commonly available in a galvanic plant operation laboratory. Furthermore, the formation of the passivation layer continuously consumes chromium, which shifts the ratio NO - 3 / Cr 3+ . The operation of the solution, which requires a tight NO - 3 / Cr 3+ ratio, thereby becomes unstable.
  • the solution also contains complexing agents from the group of monocarboxylic acids, dicarboxylic acids, tricarboxylic acids, hydroxycarboxylic acids or aminocarboxylic acids. These form partially stable complexes with the metal ions contained in the solution. These cause difficulties in wastewater treatment and are therefore undesirable.
  • EP 1 571 238 A1 describes a Cr (III) -containing passivating solution containing Cr (III) ions and at least two types of ions selected from sulfate ions, nitrate ions, chloride ions, oxyacid ions of chlorine and boron, oxyacid ions of phosphorus and fluoride ions.
  • this solution may also contain a sulfur compound.
  • Such a solution is used to make a coating for aluminum components.
  • WO 2010/035819 A1 relates to a passivation solution and the use of this black passivation solution.
  • the passivating solution is an aqueous solution containing a Cr (III) -containing substance, a cobalt-containing substance, a sulfur compound, an organophosphonic acid compound and, if necessary, a nickel-containing substance, the passivating solution being substantially free of Cr (VI ).
  • the present invention relates to the above-described acidic aqueous passivating solution containing Cr (III) ions, fluoride ions, nitrate ions and dithiodiglycolic acid, or a salt thereof, and a method for producing black passivation layers on zinc or zinc iron alloy layers, in which a workpiece provided with a zinc or zinc iron alloy layer is brought into contact with the passivation solution of the present invention. Moreover, the present invention relates to a black passivation layer obtainable by the method according to this invention.
  • the passivation solution contains a dithiodiglycolic acid (HOOC-CH 2 -SS-CH 2 -COOH) or a salt of this acid.
  • a dithiodiglycolic acid HOOC-CH 2 -SS-CH 2 -COOH
  • Any salts of dithiodiglycolic acid can be used. Examples of these are the sodium or disodium salt, the potassium or dipotassium salt and the ammonium or diammonium salt. Particularly preferred is the use of the diammonium salt of dithiodiglycolic acid.
  • the passivation solution according to the invention contains the dithiodiglycolic acid or a salt of this acid in a concentration, based on the free acid, of preferably 2-10 g / l of passivating solution, more preferably 4-6 g / l of passivating solution.
  • Cr (III) ions all soluble chromium (III) compounds can be used. Examples which may be mentioned are chromium (III) chloride, CrCl 3 .H 2 O, basic chromium (III) sulfate, CrOHSO 4 , potassium chromium sulfate, KCr (SO 4 ) 2 .6H 2 O and chromium nitrate, Cr (NO 3 ). 3 x 9H 2 O. Preferred is chromium nitrate, Cr (NO 3 ) 3 .9H 2 O.
  • the Cr (III) ions are present in the passivation solution in an amount of 1-10 g / l passivating solution, more preferably 4-5 g / l passivating solution.
  • the passivating solution according to this invention contains fluoride ions.
  • the fluoride ions are present in the passivation solution in an amount of 0.3-3 g / l passivating solution, more preferably 1-1.5 g / l passivating solution.
  • fluoride ions all soluble fluoride compounds can be used. Preferred are sodium fluoride, NaF, potassium fluoride, KF, ammonium fluoride, NH 4 F, sodium bifluoride, NaF ⁇ HF, potassium bifluoride, KF ⁇ HF, ammonium bifluoride, NH 4 F ⁇ HF. Very particularly preferred is the use of sodium fluoride, NaF.
  • the passivation solution according to the present invention also contains nitrate ions.
  • the amount of nitrate ion is 3-35 g / l passivating solution, more preferably 15-25 g / l.
  • the nitrate ions can be added to the passivating solution in any form of soluble nitrate salt. It is also possible to use a combination of several different soluble nitrate salts.
  • the nitrate ions may be added together with the Cr (III) ions as the chromium nitrate, Cr (NO 3 ) 3 .9H 2 O.
  • Another suitable nitrate salt is, for example, sodium nitrate.
  • the nitrate ion addition is in the form of sodium nitrate, it should be considered in terms of the preferred total nitrate concentration in which form the addition of the chromium compound occurs.
  • a passivating solution which comprises Cr (III) ions in an amount of 1-10 g / l passivating solution, fluoride ions in an amount of 0.3-3 g / l passivating solution, nitrate ions in an amount of 3 - 35 g / l passivation solution and dithiodiglycolic acid or a salt thereof in an amount, based on dithiodiglycolic acid, of g / l.
  • an acidic, aqueous passivating solution containing the following constituents is very particularly preferred: Cr (III) ions in an amount of 4-5 g / l passivating solution, fluoride ions in an amount of 1-1.5 g / Passivation solution, nitrate ions in an amount of 15-25 g / l passivating solution and dithiodiglycolic acid or a salt thereof in an amount, based on dithiodiglycolic acid, of 4-6 g / l.
  • the passivation solution of the present invention may contain cobalt ions.
  • the incorporation of cobalt ions in passivations based on trivalent chromium compounds is known and serves to further improve the corrosion resistance.
  • the concentration of cobalt ions in the passivating solution is preferably 0.1-10 g / l passivating solution, more preferably 0.5-5 g / l.
  • the addition of the cobalt ions can be carried out in any form of water-soluble cobalt salts. Preference is given to cobalt sulfate, cobalt chloride or cobalt nitrate.
  • the pH of the passivating solution of the present invention is suitably adjusted to a preferred range of 1.8 to 2.2, more preferably 1.9 to 2.1.
  • the present invention further provides a process for producing black passivation layers on zinc and zinc iron layers using the passivation solution described above.
  • a workpiece provided with a zinc or zinc iron layer is brought into contact with the passivating solution.
  • the contacting may be spraying, swelling or dipping.
  • dipping is used in the art.
  • the reaction temperature is preferably 10 to 70 ° C. Particularly preferred is a temperature range of 15-50 ° C, more preferably 20-50 ° C.
  • the workpieces are with the Passivation for a period of preferably 60- 90 seconds, more preferably 75 seconds, brought into contact. That is, when the workpieces are dipped in the passivation solution, the dipping time is preferably 60-90 seconds.
  • the black passivation layer may be formed on a zinc or zinc iron alloy layer.
  • a sealing layer a so-called “topcoat”
  • a sealing layer is known and improves corrosion resistance.
  • the workpiece is brought into contact with a sealing solution.
  • a sealing solution It is an aqueous solution containing organic, water-soluble or dispersible polymers.
  • organic, water-soluble or dispersible polymers For example, copolymers of acrylic acid or methacrylic acid with ethylene, commercially available under the name Lugalavan DC Fa. BASF, are used.
  • Inorganic sealant solutions contain colloidal silicic acids. It is also possible to prepare mixtures of aqueous solutions with organic polymers and aqueous solutions with colloidal silicas and to use these as a sealing solution.
  • the present invention also provides a black passivation layer obtainable by the method described above.
  • the black passivation layer is formed on a pure zinc layer.
  • the mixture is heated to 65 ° C for 30 minutes, then cooled to room temperature. It is then made up to 1 liter with deionized water.
  • the volume was made up to approximately 1 liter with deionized water, then the pH was reduced with conc. Nitric acid (53 wt.%) Adjusted to 1.8 to 1.9 and made up to the final volume of 1 liter.
  • test sheet was rinsed in deionized water, immersed in dilute nitric acid solution (10 ml / l HNO 3 53% by weight) for 5 seconds and then in the above immersed in the following conditions: Temperature: 25 ° C PH value: 1.8 - 1.9 Dive time: 60 seconds
  • test sheet was then rinsed with deionized water and dried in a drying oven at 80 ° C for 15 minutes. The appearance of the test sheet was then deep black with slightly brownish iridescent spots.
  • Example 1 was repeated as described. After passivation and rinsing, it was immersed in a sealing solution (SLOTOFIN 70 from Dr.-Ing. Max Schlötter, aqueous dispersion of a copolymer of acrylic acid and ethylene).
  • SLOTOFIN 70 from Dr.-Ing. Max Schlötter, aqueous dispersion of a copolymer of acrylic acid and ethylene.
  • test sheet was dried without rinsing at 80 ° C for 15 minutes in a drying oven.
  • the sealed test sheet had a uniform deep black, semi-glossy appearance.
  • Test panels which were prepared according to Examples 1 and 2, were tested in a corrosion test in the neutral salt spray test according to DIN EN ISO 9227. Following DIN 50 979, 1 sample was tested without additional heat treatment and 1 sample was annealed at 120 ° C. for 24 hours. corrosion protection without heat treatment with heat treatment (120 ° C / 24h) example 1 72 h 72 h Example 2 > 240 h > 240 h
  • the volume was made up to approximately 1 liter with deionized water, then the pH was reduced with conc. Nitric acid (53 wt.%) Adjusted to 1.8 to 1.9 and made up to the final volume of 1 liter.
  • a passivation solution was prepared as in Comparative Example 1, but thiodiglycolic acid was replaced by 4 g of cystine. The passivation reaction did not result in blackening.

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

Claims (6)

  1. Solution de passivation aqueuse acide pour la production de couches de passivation noires sur des couches de zinc ou d'alliage de zinc et de fer, contenant
    - des ions Cr(III),
    - des ions fluorure et
    - des ions nitrate,
    caractérisée en ce que la solution de passivation contient en plus un acide dithiodiglycolique ou un sel dudit acide, et la solution de passivation contenant
    - des ions Cr(III) en une quantité de 1 à 10 g/l de solution de passivation,
    - des ions fluorure en une quantité de 0,3 à 3 g/l de solution de passivation,
    - des ions nitrate en une quantité de 3 à 35 g/l de solution de passivation et
    - un acide dithiodiglycolique ou un sel de ce dernier en une quantité, par rapport à l'acide dithiodiglycolique, de 2 à 10 g/l.
  2. Solution de passivation selon la revendication 1, la solution de passivation présentant une valeur de pH de 1,8 à 2,2.
  3. Procédé pour la production de couches de passivation noires sur une couche de zinc ou d'alliage de zinc et de fer, caractérisé en ce qu'une pièce revêtue d'une couche de zinc ou d'alliage de zinc et de fer est amenée en contact avec la solution de passivation aqueuse acide selon l'une quelconque ou plusieurs des revendications 1 à 2.
  4. Procédé selon la revendication 3, la pièce étant amenée en contact avec la solution de passivation à une température de réaction de 10 - 70 °C.
  5. Procédé selon la revendication 3 ou 4, la pièce étant amenée en contact avec la solution de passivation pour une durée de 60 - 90 secondes.
  6. Procédé selon l'une quelconque ou plusieurs des revendications 3 à 5, la couche de passivation noire étant formée sur une couche de zinc pur.
EP10175959.5A 2009-10-12 2010-09-09 Passivation noire de zinc et couches de fer et de zinc Active EP2319957B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SI201031381A SI2319957T1 (sl) 2009-10-12 2010-09-09 Črna pasivacija cinkovih in cinkovo-železovih plasti

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102009045569A DE102009045569A1 (de) 2009-10-12 2009-10-12 Schwarzpassivierung von Zink- und Zinkeisenschichten

Publications (2)

Publication Number Publication Date
EP2319957A1 EP2319957A1 (fr) 2011-05-11
EP2319957B1 true EP2319957B1 (fr) 2017-01-11

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Application Number Title Priority Date Filing Date
EP10175959.5A Active EP2319957B1 (fr) 2009-10-12 2010-09-09 Passivation noire de zinc et couches de fer et de zinc

Country Status (4)

Country Link
EP (1) EP2319957B1 (fr)
DE (1) DE102009045569A1 (fr)
DK (1) DK2319957T3 (fr)
SI (1) SI2319957T1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2784188B2 (fr) 2013-03-26 2018-04-25 ATOTECH Deutschland GmbH Procédé de protection contre la corrosion de matériaux contenant du fer
CN103741128B (zh) * 2014-01-06 2016-01-20 哈尔滨三泳金属表面技术有限公司 电镀锌层高耐蚀三价铬彩色钝化剂
DE102016114808B4 (de) * 2016-08-10 2023-06-07 Harting Electric Stiftung & Co. Kg Steckverbinder mit vor Korrosion geschütztem Steckverbindergehäuse

Family Cites Families (9)

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Publication number Priority date Publication date Assignee Title
GB1532230A (en) * 1975-11-24 1978-11-15 Imasa Ltd Treatment of chromated metal surfaces with sulphur-compounds
FR2812307B1 (fr) 2000-07-25 2003-02-14 Chemetall S A Couche noire anticorrosive sur un alliage de zinc et son procede de preparation
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。
JP4508634B2 (ja) * 2003-12-26 2010-07-21 株式会社タイホー 金属表面処理剤、金属表面処理液、これによって形成された耐食性着色皮膜、この耐食性着色皮膜を有する耐食性着色部品、およびこの耐食性着色部品の製造方法
DE102004001945A1 (de) 2004-01-14 2005-08-11 Ina-Schaeffler Kg Schwarzpassivierung von Zink- oder Zinklegierungsoberflächen
JP4628726B2 (ja) * 2004-03-02 2011-02-09 日本表面化学株式会社 アルミニウム部材及びその製造方法と製造用薬剤
JP5161761B2 (ja) 2006-02-17 2013-03-13 ディップソール株式会社 亜鉛又は亜鉛合金上に黒色の３価クロム化成皮膜を形成するための処理溶液及び亜鉛又は亜鉛合金上に黒色の３価クロム化成皮膜を形成する方法
US7842403B2 (en) * 2006-02-23 2010-11-30 Atotech Deutschland Gmbh Antifriction coatings, methods of producing such coatings and articles including such coatings
EP2336390B1 (fr) * 2008-09-29 2014-07-30 Yuken Industry Co., Ltd. Composition pour traitement de transformation chimique et procédé de production d un élément pourvu d un revêtement noir à l aide de ladite composition

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Also Published As

Publication number Publication date
DE102009045569A1 (de) 2011-04-14
EP2319957A1 (fr) 2011-05-11
DK2319957T3 (en) 2017-02-27
SI2319957T1 (sl) 2017-05-31

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