EP0328908B1 - Procédé pour appliquer des couches de conversion - Google Patents

Procédé pour appliquer des couches de conversion Download PDF

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Publication number
EP0328908B1
EP0328908B1 EP89101302A EP89101302A EP0328908B1 EP 0328908 B1 EP0328908 B1 EP 0328908B1 EP 89101302 A EP89101302 A EP 89101302A EP 89101302 A EP89101302 A EP 89101302A EP 0328908 B1 EP0328908 B1 EP 0328908B1
Authority
EP
European Patent Office
Prior art keywords
solution
metal surfaces
brought
contact
ppm
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 - Lifetime
Application number
EP89101302A
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German (de)
English (en)
Other versions
EP0328908A1 (fr
Inventor
George Leonard Higgins
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.)
GEA Group AG
Chemetall Ltd
Original Assignee
Metallgesellschaft AG
Brent Chemicals International PLC
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 Metallgesellschaft AG, Brent Chemicals International PLC filed Critical Metallgesellschaft AG
Publication of EP0328908A1 publication Critical patent/EP0328908A1/fr
Application granted granted Critical
Publication of EP0328908B1 publication Critical patent/EP0328908B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • C23C22/60—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 alkaline aqueous solutions with pH greater than 8
    • C23C22/66—Treatment of aluminium or alloys based thereon
    • C23C22/67—Treatment of aluminium or alloys based thereon with solutions containing hexavalent chromium
    • 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
    • C23C22/60—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 alkaline aqueous solutions with pH greater than 8

Definitions

  • the invention relates to a method for applying conversion coatings on metal surfaces made of aluminum, zinc and their alloys with the aid of solutions containing alkaline ChromVI and ChromIII.
  • the concentration of the hexavalent chromium is approximately 13 g / l (expressed as CrO3), but the concentration of the dissolved trivalent chromium is extremely low, approximately in the order of 1 ppm, even if the solution is saturated with chromium III oxide. The reason is the very low solubility of the trivalent chromium at high pH values of the solution.
  • the relatively thick conversion coating obtained by this process consists essentially of aluminum and chromium III oxide.
  • the aforementioned method has numerous disadvantages.
  • the appearance of the conversion coating formed is very different, for example stained or marbled green and / or brown.
  • the treatment requires a diving time of about 5 minutes at a temperature of 90 to 100 ° C.
  • the high content of hexavalent chromium in the solution requires extensive treatment of the waste water.
  • GB-PS 899 599 provides for essentially colorless chromate coatings on surfaces of zinc or conventional zinc alloys by treatment with a strongly acidic (pH 0.2 to 2.8) solution containing hexavalent chromium and trivalent chromium produce.
  • concentration of the hexavalent chromium is around 10 g / l (calculated as chromium VI oxide) and is therefore also complex with regard to the required wastewater treatment.
  • the strongly acidic reaction of the chromating solution also makes the solution very aggressive, so that material suitable for plant construction is only available to a limited extent.
  • this method cannot be used satisfactorily for the treatment of aluminum, since acidic solutions tend to be somewhat ineffective on aluminum if they do not contain fluoride.
  • the use of solutions containing acid fluoride in turn leads to unsatisfactory results in the treatment of zinc.
  • GB-PS 1 042 108 describes a method for the treatment of zinc and conventional zinc alloys, in which the zinc surfaces are treated with a chromium VI-free aqueous alkaline solution, the pH of which is above 11 and which is one of the Group 1 of the periodic system contains different metal, brought into contact.
  • the majority of the examples show the use of metals such as iron, cobalt or magnesium, whereas trivalent chromium is not mentioned as a suitable metal.
  • the use of hexavalent chromium is expressly excluded, since it allegedly affects the formation of the desired conversion coating.
  • DE-A1-37 11 095 is a method for producing conversion coatings on Zn or Zn alloy surfaces by means of aqueous solutions, the Cr (III) ions and ions of at least two other multivalent metals, preferably Fe (III) ions, and Contains Co and / or Ni ions and complexing agents and whose pH is greater than 11, known.
  • the object of the invention is to provide a method which allows the treatment of pure aluminum, pure zinc, but also of alloys of zinc or aluminum with other metals, but in particular the treatment of zinc / aluminum alloys using the same solutions.
  • the object is achieved by designing the method of the type mentioned at the outset in accordance with the invention in such a way that the metal surfaces are brought into contact with a solution which, owing to the addition of a Complexing agent for ChromIII contains at least 20 ppm dissolved ChromIII.
  • the complexing agent can be used to adjust the concentrations of the chromium III to such considerably higher values.
  • the hexavalent chromium can be introduced into the treatment solutions in the form of suitable soluble chromates, preferably as alkali chromates. If the concentration of hexavalent chromium is too low, the required conversion coating does not take place, so that the protection achieved is inadequate. If the concentrations are too high, there is a tendency to passivate the metal surfaces instead of forming a conversion coating formed by reaction.
  • the metal surfaces are brought into contact with a solution which contains 8 to 75 ppm of ChromVI. It is particularly advantageous to bring the metal surfaces into contact with a solution that contains 15 to 60 ppm ChromVI.
  • the trivalent chromium can be added as any suitable soluble chromium compound, especially as a chromium salt.
  • the conversion coating produced by the process according to the invention is usually rinsed with water, it is desirable to use a salt with an anion which does not cause any corrosion problems.
  • a further advantageous embodiment of the invention therefore provides for the metal surfaces to be brought into contact with a solution in which the chromium III is introduced as nitrate, sulfate, phosphate and / or acetate.
  • Halides, especially chlorides should preferably not be used.
  • chromium III carbonate can also be used, but this requires the presence of an initially acidic solution, which is then made alkaline by adding alkali.
  • Another way of achieving the required chromium III content in the solution is to produce it by reducing the excess hexavalent chromium which has previously been introduced.
  • the reduction required for this usually takes place in an acidic medium, so that alkali must subsequently be added.
  • the reduction can, for example, be brought about by introducing organic reducing agents into the solution in a manner known per se.
  • the concentration of trivalent chromium is below 30 ppm, the conversion coating can be formed relatively slowly. Accordingly, an advantageous development of the invention provides for the metal surfaces to be brought into contact with a solution which contains at least 30 ppm, preferably even at least 50 ppm, of chromium III. It is particularly advantageous to adjust the concentration of trivalent chromium to a maximum of 700 ppm, preferably to 100 to 500 ppm. At concentrations above 700 ppm, no further advantages are usually achieved.
  • the pH of the solution should be above 12, otherwise the process takes place with too slow a coating formation.
  • the setting of a pH value of at least 12.5 is particularly advantageous.
  • the pH value is usually determined by a suitable one which does not impair the formation of the coating Alkali made.
  • the use of sodium silicate should be avoided, since a sodium silicate content tends to passivate individual surfaces, particularly those made of aluminum.
  • Sodium carbonate can be used, but the required pH cannot be achieved with it, so that additional pH adjustment with alkali hydroxide is required. It is therefore most expedient to use alkali hydroxide, in particular sodium and / or potassium hydroxide, for the entire pH adjustment.
  • the amount of the hydroxides is generally at least 10 g / l, but is below 80 g / l. If the concentration is too high, there is a risk that the solution will vigorously etch the zinc and aluminum surface and fail to provide the desired coating.
  • any compound capable of keeping the required amounts of trivalent chromate in solution can be used as the complexing agent.
  • the metal surfaces are brought into contact with a solution which is used as a complexing agent for chromium III hydroxycarboxylic acid, in particular gluconic acid and / or hexahydroxy heptanoic acid, such as glucoheptanoic acid, or but contains as a complexing agent for ChromIII aminocarboxylic acid, in particular nitrilotriacetic acid and / or ethylenediaminetetraacetic acid.
  • Citric acid is suitable as the hydroxy carboxylic acid, albeit less advantageously.
  • the aforementioned acids can also be introduced into the solution in the form of their sodium salts.
  • aminocarboxylic acid especially in combination with hydroxycarboxylic acid, has the advantage that the effectiveness of the method is increased by a more uniform pickling attack on the metal surface and the formation of a particularly uniform conversion coating.
  • the metal surfaces are brought into contact with a solution which contains the hydroxycarboxylic acid in an amount of 0.2 to 10 g / l or the aminocarboxylic acid in an amount of 0.5 to 10 g / l .
  • the aforementioned quantities refer to the neutral sodium salts.
  • the solution required to carry out the method according to the invention can be prepared by dissolving the individual constituents in water while adjusting the concentrations required in each case.
  • the alkali required for pH adjustment can be added separately or already contained in the batch concentrate.
  • Suitable concentrates usually have a solids content of 15 to 40% by weight, in particular 25 to 35% by weight. They contain the effective solution components in the ratio in which they are also contained in the working solution. This makes it possible to prepare the working solution by simply diluting it with the appropriate amount of water.
  • the method according to the invention can be applied in any known manner, the treatment of the metal surfaces in spraying or immersion is preferred.
  • the treatment time can be very short, for example 5 to 15 s, but longer treatment times, for example up to 1 minute, are also possible. The latter applies in particular when the concentration of trivalent chromium and / or the treatment temperatures are comparatively low.
  • the temperature of the solution to be brought into contact with the metal surface is normally below 70 ° C, generally in the range of 40 to 60 ° C.
  • the workpieces to be treated are generally at a temperature of 30 to 50 ° C, usually at about 40 ° C before treatment.
  • the conversion coating formed by the process according to the invention is generally rinsed with water, generally by spraying. Furthermore, it is advantageous to carry out a passivation rinse with a chromate solution, preferably as described in GB-PS 1 084 478, following the application of the conversion coating. This is followed by drying.
  • the conversion coatings produced with the method according to the invention have good corrosion resistance. You can stay without further post-treatment, but in general it is common to apply a varnish afterwards, which can be both colorless and colored.
  • the method according to the invention is advantageously applicable to the treatment of zinc, aluminum and their alloys with other metals or with one another.
  • the invention is particularly advantageous if the intention is to treat different metal surfaces simultaneously or subsequently.
  • hot-dip galvanized or hot-dip galvanized steel strip can be treated without having to change the nature of the solution.
  • the aforementioned solution was sprayed on at 50 ° C. for 15 seconds onto steel strip which was hot-dip galvanized or hot-dip coated with a zinc / aluminum alloy.
  • the alloy consisted of 5% by weight aluminum and 95% by weight zinc. Following the conversion treatment, it was rinsed with water in a syringe and dried. An epoxy primer and a top coat made of a silicone-modified polyester were then applied.
  • the steel strip treated in this way was treated in the salt spray test in accordance with ASTM-B 117 for a period of 1500 h. The subsequent evaluation showed that, based on the cross-cut, the paint had infiltrated ⁇ 1 mm.
  • a concentrate was made that contains, manufactured.
  • a working solution can be prepared from the aforementioned concentrate by dilution with water in a ratio of 1:10.

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  • 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)
  • Application Of Or Painting With Fluid Materials (AREA)

Claims (10)

1. Procédé pour l'application de couches de conversion sur des surfaces métalliques en aluminium, zinc et leur alliages, à l'aide de solutions alcalines contenant du chrome-VI et du chrome-III, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient, par suite de l'addition d'un complexant pour le chrome-III, au moins 20 ppm de chrome-III dissous.
2. Procédé selon la revendication 1, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient de 8 à 75 ppm, de préférence de 15 à 60 ppm de chrome-VI.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution dans laquelle le chrome-III est introduit sous forme de nitrate, sulfate, phosphate et/ou acétate.
4. Procédé selon la revendication 1, 2 ou 3, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient au moins 30 ppm, de préférence au moins 50 ppm de chrome-III.
5. Procédé selon une ou plusieurs des revendications 1 à 4, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient au maximum 700 ppm, de préférence de 100 à 500 ppm, de chrome-III.
6. Procédé selon une ou plusieurs des revendications 1 à 5, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution dont le pH est au moins 12, de préférence au moins 12,5.
7. Procédé selon une ou plusieurs des revendications 1 à 6, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient, en tant que complexant pour le chrome-III, un acide hydroxycarboxylique, en particulier l'acide gluconique, et/ou un acide hexahydroxyheptanoïque, tel que l'acide glucoheptanoïque.
8. Procédé selon une ou plusieurs des revendications 1 à 7, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient, en tant que complexant pour le chrome-III, un acide aminocarboxylique, en particulier l'acide nitrilotriacétique et/ou l'acide éthylènediaminetétraacétique.
9. Procédé selon la revendication 7, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient l'acide hydroxycarboxylique en une quantité de 0,2 à 10 g/l.
10. Procédé selon la revendication 8, caractérisé en ce que l'on met les surfaces métalliques en contact avec une solution qui contient l'acide aminocarboxylique en une quantité de 0,5 à 10 g/l.
EP89101302A 1988-02-08 1989-01-26 Procédé pour appliquer des couches de conversion Expired - Lifetime EP0328908B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB888802788A GB8802788D0 (en) 1988-02-08 1988-02-08 Composition & process for treating metal surfaces
GB8802788 1988-02-08

Publications (2)

Publication Number Publication Date
EP0328908A1 EP0328908A1 (fr) 1989-08-23
EP0328908B1 true EP0328908B1 (fr) 1992-03-04

Family

ID=10631278

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89101302A Expired - Lifetime EP0328908B1 (fr) 1988-02-08 1989-01-26 Procédé pour appliquer des couches de conversion

Country Status (8)

Country Link
US (1) US4963198A (fr)
EP (1) EP0328908B1 (fr)
JP (1) JPH01283386A (fr)
AU (1) AU614024B2 (fr)
DE (2) DE3902266A1 (fr)
ES (1) ES2031288T3 (fr)
GB (1) GB8802788D0 (fr)
NZ (1) NZ227807A (fr)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5223028A (en) * 1991-08-19 1993-06-29 Lexmark International, Inc. Waterfast aqueous inks
US6461449B1 (en) 1997-10-07 2002-10-08 Henkel Corporation Conversion coating zinciferous surfaces to resist blackening and white rust
JPH11106944A (ja) * 1997-10-07 1999-04-20 Nippon Parkerizing Co Ltd 耐黒変性及び耐白錆性に優れた亜鉛系めっき鋼板の製造方法
DE60000519T2 (de) 1999-02-25 2003-01-30 Ngk Spark Plug Co Glühkerze und Zündkerze, und ihr Herstellungsverfahren
US6375726B1 (en) 2000-10-31 2002-04-23 The United States Of America As Represented By The Secretary Of The Navy Corrosion resistant coatings for aluminum and aluminum alloys
US6663700B1 (en) * 2000-10-31 2003-12-16 The United States Of America As Represented By The Secretary Of The Navy Post-treatment for metal coated substrates
US6527841B2 (en) * 2000-10-31 2003-03-04 The United States Of America As Represented By The Secretary Of The Navy Post-treatment for metal coated substrates
US6511532B2 (en) * 2000-10-31 2003-01-28 The United States Of America As Represented By The Secretary Of The Navy Post-treatment for anodized aluminum
US6521029B1 (en) * 2000-10-31 2003-02-18 The United States Of America As Represented By The Secretary Of The Navy Pretreatment for aluminum and aluminum alloys
US6669764B1 (en) * 2000-10-31 2003-12-30 The United States Of America As Represented By The Secretary Of The Navy Pretreatment for aluminum and aluminum alloys
DE102005059748B4 (de) * 2005-06-15 2020-03-19 Continental Teves Ag & Co. Ohg Verfahren zur Verdichtung anodisch oxidierter Aluminiumwerkstücke
US8092617B2 (en) * 2006-02-14 2012-01-10 Henkel Ag & Co. Kgaa Composition and processes of a dry-in-place trivalent chromium corrosion-resistant coating for use on metal surfaces
RU2434972C2 (ru) * 2006-05-10 2011-11-27 ХЕНКЕЛЬ АГ унд Ко. КГаА. Улучшенная, содержащая трехвалентный хром композиция для применения в коррозионно-стойких покрытиях на металлических поверхностях
KR100872479B1 (ko) 2007-03-27 2008-12-15 (주)하나나노텍 3가 크로메이트 용액과 3가 크로메이트 처리된 금속체 및그의 제조방법
US10156016B2 (en) 2013-03-15 2018-12-18 Henkel Ag & Co. Kgaa Trivalent chromium-containing composition for aluminum and aluminum alloys
JP6396563B1 (ja) * 2017-10-10 2018-09-26 奥野製薬工業株式会社 表面処理液

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB441088A (en) * 1934-07-13 1936-01-13 Pyrene Co Ltd Improvements relating to the production of protective or paintholding coatings on aluminium or aluminium alloys
US2911332A (en) * 1956-05-25 1959-11-03 Kelsey Hayes Co Process of coating metal and resulting articles
GB869395A (en) * 1959-05-27 1961-05-31 Pyrene Co Ltd Improvements relating to the production of chemical coatings on zinc and zinc alloys
BE635940A (fr) * 1962-08-15
SE316668B (fr) * 1963-09-23 1969-10-27 Parker Ste Continentale
US3935035A (en) * 1973-06-05 1976-01-27 Nippon Steel Corporation Aqueous solution and method for surface treatment of metals
GB8608508D0 (en) * 1986-04-08 1986-05-14 Pyrene Chemical Services Ltd Coating metal surfaces

Also Published As

Publication number Publication date
DE3902266A1 (de) 1989-08-17
US4963198A (en) 1990-10-16
AU2969189A (en) 1989-08-10
ES2031288T3 (es) 1992-12-01
NZ227807A (en) 1991-08-27
AU614024B2 (en) 1991-08-15
DE58900881D1 (de) 1992-04-09
JPH01283386A (ja) 1989-11-14
EP0328908A1 (fr) 1989-08-23
GB8802788D0 (en) 1988-03-09

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