EP0213590B1 - Verfahren zur Erzeugung von Konversionsschichten auf Zink und/oder Zink/Aluminium-Legierungen - Google Patents

Verfahren zur Erzeugung von Konversionsschichten auf Zink und/oder Zink/Aluminium-Legierungen Download PDF

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Publication number
EP0213590B1
EP0213590B1 EP86111789A EP86111789A EP0213590B1 EP 0213590 B1 EP0213590 B1 EP 0213590B1 EP 86111789 A EP86111789 A EP 86111789A EP 86111789 A EP86111789 A EP 86111789A EP 0213590 B1 EP0213590 B1 EP 0213590B1
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EP
European Patent Office
Prior art keywords
zinc
ions
chromating
solution
weight
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
EP86111789A
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German (de)
English (en)
French (fr)
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EP0213590A1 (de
Inventor
Gary A. Reghi
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Henkel Corp
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Henkel Corp
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Filing date
Publication date
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Priority to AT86111789T priority Critical patent/ATE65266T1/de
Publication of EP0213590A1 publication Critical patent/EP0213590A1/de
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Publication of EP0213590B1 publication Critical patent/EP0213590B1/de
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
    • C23C22/06—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
    • 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
    • C23C22/40—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 molybdates, tungstates or vanadates
    • C23C22/44—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 molybdates, tungstates or vanadates containing also 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
    • C23C22/24—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 hexavalent chromium compounds
    • C23C22/33—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 hexavalent chromium compounds containing also phosphates
    • 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
    • C23C22/37—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 containing also hexavalent chromium compounds
    • C23C22/38—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 containing also hexavalent chromium compounds containing also phosphates

Definitions

  • the invention relates to a process for the production of conversion layers on surfaces made of zinc and / or zinc-aluminum alloys by means of aqueous acidic chromating solutions which contain chromium VI, nitrate and phosphate ions.
  • the chromating solution contains 0.1 to 15 g / l Cr6+, 1.0 to 12 g / l Cl ⁇ , 0.5 to 2.0 g / l F ⁇ , 0.5 to 2.0 g / l SO42 ⁇ , 0.5 to 3.0 g / l Zn2+ and optionally 0.05 to 1.0 g / l PO43 ⁇ and 0.005 to 1.0 g / l NO3 ⁇ .
  • a zinc alloy containing 1 to 30% by weight of aluminum is treated to form chromate.
  • US Pat. No. 4,531,978 discloses a process for producing chromate conversion coatings on aluminum surfaces, the aluminum surface being immersed in an acidic, aqueous solution which contains hexavalent chromium. In addition, the aluminum surface is subjected to an ultrasound treatment to avoid the commonly used accelerator components.
  • the sheets are placed in an aqueous solution containing 0.005 to 1 mol / l chromium anhydride, 0.001 to 0.5 mol / l nickel, cobalt and iron as nitrate, sulfate, phosphate, fluoride or as a fluorocomplex.
  • the object of the invention is to provide a process for producing conversion layers which, particularly when used on zinc-aluminum alloys, gives good results in terms of corrosion resistance, but is also universally applicable insofar as conventional "pure" zinc surfaces are provided with a conversion layer can be.
  • 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 surfaces are brought into contact with a chloride-free chromating solution which contains 2 to 20 g / l of chromium ions (calculated as Cr) and 1 to 15 g / l phosphate ions (calc. as PO4) and 0.5 to 6 g / l nitrate ions (calc. as NO3) contains.
  • the process is for the treatment of zinc surfaces, i.e. Workpieces made of solid zinc, or galvanized metals, such as galvanized steel, which contain practically no or only minor alloy components, but in particular for surfaces made of zinc-aluminum alloy, e.g. of the aforementioned quality.
  • the active constituents of the chromating solution are introduced in a manner known per se.
  • the chromium VI ions are expediently added via chromic acid, alkali metal or ammonium chromate or dichromate.
  • the chromating solution generally also contains chromium III ions, which can be added as such or can be generated by reducing some of the chromium VI ions.
  • the major part of the chromium ions dissolved in the chromating solution is in the hexavalent state.
  • nitrate ions are most conveniently introduced via nitric acid, alkali and / or ammonium nitrate.
  • nitric acid alkali and / or ammonium nitrate.
  • the use of nitric acid is preferred.
  • the phosphate ion content is adjusted in the simplest manner by adding alkali metal or ammonium phosphate or polyphosphate or else by adding phosphoric acid.
  • the chromating solution works in the acidic range. It is particularly advantageous to bring the surfaces into contact with a chromating solution whose pH is below 2.
  • the pH can be adjusted if individual of the aforementioned bath components are added in the form of free acid. However, other suitable acids can also be used.
  • a further preferred embodiment of the invention therefore provides for the surfaces to be brought into contact with a chromating solution which additionally contains an amount of fluoride, preferably 0.5 g / l, or molybdate, preferably 0.5 to 0.7 g, which accelerates the formation of the layer / l, or tungsten, preferably about 0.2 g / l.
  • the fluoride is expediently added in the form of hydrofluoric acid, molybdate in the form of the alkali or ammonium salt, tungstate in the form of alkali tungstate.
  • the treatment solution is applied to the previously cleaned surfaces in the usual way, for example by spraying, dipping, flooding, brushing or roller application. Excess solution can be removed, for example by using squeeze rollers. In this way, a liquid film with a certain thickness is created on the surface, which - when it dries - is responsible for the desired layer weight.
  • the layer weight should be set to approximately 10.8 mg / m 2 (calculated as Cr). In processes in which the layer is formed in contact with the chromating solution, the layer weight obtained depends on the duration of the treatment, the temperature of the chromating solution and the concentration of the active ingredients.
  • the application temperature of the chromating solution is generally in the range from 37.8 to 87.8 ° C. A temperature in the interval of 54.4 to 71.1 ° C is preferred. A treatment temperature of 60 ° C. is particularly favorable.
  • the treatment time can be between 0.5 sec. And 1 min. lie. If particularly high layer weights are desired, the treatment time can also be over 1 min. lie.
  • the process for the production of galvanized and chromated steel strip usually proceeds as follows: The steel strip is first cleaned with an organic solvent to remove anti-rust oil, then subjected to cleaning with, for example, an alkaline cleaner. This is followed by water rinsing, drying and galvanizing in a zinc-aluminum alloy melt. After the alloy layer has solidified, the strip can be brought into direct contact with the chromating solution.
  • the chromating solution can be prepared directly in a usable form using the effective bath components. In general, however, it is more expedient to prepare the treatment solution using a concentrate.
  • a suitable concentrate contains, for example, 30.4% by weight chromic acid (approx. 219 g / l chromium ions); 4.35% by weight nitric acid (100% by weight; approx. 59 g / l nitrate ions), 10.65% by weight phosphoric acid (100% by weight; approx. 142 g / l phosphate ions), Rest of water. It has a density of 1.383 g / cm3.
  • the sheet obtained in this way was cut into sheet pieces measuring 9 x 19 cm and oiled with an anti-rust oil (Castrol Rustillo® DW-924 HF).
  • the pieces of sheet metal were then subjected to the industry standard test to determine weather resistance.
  • the rust protection oil was first removed with petroleum solvent.
  • the sheet metal pieces were placed upright in glass dishes filled with distilled water in a damp room which had been heated to 37.7 ° C.
  • the appearance of the surface was checked and assessed at regular intervals with regard to darkening or discoloration.
  • the evaluation was carried out on a scale ranging from 1 to 8, with 8 meaning no discernible and 1 complete darkening. The results are shown in the table below.
  • a second series of sheet metal pieces was treated and tested as indicated in Example 1.
  • a third series of sheet metal pieces was treated and evaluated as indicated in Example 1.
  • a conventional chromating solution the 0.38% by weight chromic acid 0.11% by weight boric acid 0.11% by weight of hydrofluoric acid (70% by weight) contained.
  • a fourth series of sheet metal pieces was treated and evaluated as described in Example 1, but treatment with a chromating solution was omitted.
  • Example 4 The results show that the merely cleaned sheet metal pieces (Example 4) were completely dark after a test period of 168 hours. In contrast, the sheet metal pieces treated according to Example 1 had a rating of 7.5 after a test duration of 1100 hours. The sheet metal pieces treated in accordance with Example 2 even received the grade 8 corresponding to no discernible discoloration. Even with a test duration of 2164 hours, the sheet metal pieces with marks of 7.3 (example 1) or 7.8 (example 2) were still of excellent quality.

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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)
  • Prevention Of Electric Corrosion (AREA)
  • Laminated Bodies (AREA)
EP86111789A 1985-09-06 1986-08-26 Verfahren zur Erzeugung von Konversionsschichten auf Zink und/oder Zink/Aluminium-Legierungen Expired - Lifetime EP0213590B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86111789T ATE65266T1 (de) 1985-09-06 1986-08-26 Verfahren zur erzeugung von konversionsschichten auf zink und/oder zink/aluminium-legierungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US77340585A 1985-09-06 1985-09-06
US773405 1985-09-06

Publications (2)

Publication Number Publication Date
EP0213590A1 EP0213590A1 (de) 1987-03-11
EP0213590B1 true EP0213590B1 (de) 1991-07-17

Family

ID=25098170

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86111789A Expired - Lifetime EP0213590B1 (de) 1985-09-06 1986-08-26 Verfahren zur Erzeugung von Konversionsschichten auf Zink und/oder Zink/Aluminium-Legierungen

Country Status (10)

Country Link
EP (1) EP0213590B1 (xx)
JP (1) JPS6256579A (xx)
KR (1) KR870003229A (xx)
AT (1) ATE65266T1 (xx)
AU (1) AU590885B2 (xx)
CA (1) CA1274754A (xx)
DE (2) DE3628660A1 (xx)
ES (1) ES2001659A6 (xx)
GB (1) GB2179960B (xx)
NZ (1) NZ216539A (xx)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107513703A (zh) * 2017-08-24 2017-12-26 南通市烨达汽车零部件有限公司 一种汽车用表面金属处理剂

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8828559D0 (en) * 1988-12-07 1989-01-11 Novamax Tech Corp Composition & method for coating metal surfaces
GB2231063A (en) * 1989-02-27 1990-11-07 Omi International Electroless plating composition containing saccharin
NL9000310A (nl) * 1989-02-27 1990-09-17 Omi Int Corp Mengsel en werkwijze voor omzetting.
JPH055185A (ja) * 1991-06-26 1993-01-14 Nippon Parkerizing Co Ltd アルミニウムの表面処理方法
US5498759A (en) * 1991-06-26 1996-03-12 Henkel Corporation Surface treatment method for aluminum
AUPP375198A0 (en) * 1998-05-28 1998-06-18 Bhp Steel (Jla) Pty Limited An anticorrosion treatment
GB2374088A (en) * 2001-03-29 2002-10-09 Macdermid Plc Conversion treatment of zinc and zinc alloy surfaces
ES2807509T3 (es) * 2012-10-18 2021-02-23 Bluescope Steel Ltd Procedimiento de producción de banda de acero revestida con metal

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GB712691A (en) * 1950-03-07 1954-07-28 Gen Motors Corp Chemical solutions for treating metal surfaces and methods of using the same
NL107091C (xx) * 1957-01-31
NL248160A (xx) * 1959-02-09
GB984055A (en) * 1963-06-04 1965-02-24 Protime Soc Anti-corrosion product
NL6606084A (xx) * 1966-05-05 1967-11-06
GB1164726A (en) * 1967-03-24 1969-09-17 M & T Chemicals Inc Coating of Aluminium and Aluminium Alloys
US3562011A (en) * 1968-04-26 1971-02-09 Gen Electric Insulating coating comprising an aqueous mixture of the reaction product of chromium nitrate and sodium chromate,phosphoric acid and colloidal silica and method of making the same
GB1435518A (en) * 1972-10-12 1976-05-12 Int Nickel Ltd Electrolytic treatment of chromium-containing alloys and electro lytes for use therein
US3798074A (en) * 1972-03-23 1974-03-19 Allegheny Ludlum Ind Inc Surface finishing
JPS5648591B2 (xx) * 1973-11-15 1981-11-17
JPS5268036A (en) * 1975-12-04 1977-06-06 Nisshin Steel Co Ltd Process for surface treating steel sheet by phosphoric acidd0chromic acid bath
JPS5817832B2 (ja) * 1977-08-13 1983-04-09 日本ペイント株式会社 アルミニウム，亜鉛およびそれらの合金材の表面処理方法
DE2854355A1 (de) * 1978-12-15 1980-06-26 Amchem Prod Saures, waessriges mittel zur herstellung eines chromatumwandlungsueberzuges auf aluminiumhaltigen oberflaechen und verfahren zur herstellung eines chromatumwandlungsueberzuges auf aluminiumhaltigen oberflaechen
US4531978A (en) * 1983-04-11 1985-07-30 Detrex Chemical Industries, Inc. Method of forming chromate conversion coatings on aluminum surfaces and the coating formed thereby
JPS59222587A (ja) * 1983-06-02 1984-12-14 Mitsui Mining & Smelting Co Ltd クロメ−ト処理方法
JPS6026672A (ja) * 1983-07-22 1985-02-09 Mitsui Mining & Smelting Co Ltd クロメ−ト処理方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107513703A (zh) * 2017-08-24 2017-12-26 南通市烨达汽车零部件有限公司 一种汽车用表面金属处理剂

Also Published As

Publication number Publication date
DE3680263D1 (de) 1991-08-22
DE3628660A1 (de) 1987-03-19
GB2179960A (en) 1987-03-18
AU590885B2 (en) 1989-11-23
NZ216539A (en) 1989-02-24
ES2001659A6 (es) 1988-06-01
GB8621560D0 (en) 1986-10-15
JPS6256579A (ja) 1987-03-12
KR870003229A (ko) 1987-04-16
EP0213590A1 (de) 1987-03-11
GB2179960B (en) 1990-01-24
CA1274754A (en) 1990-10-02
ATE65266T1 (de) 1991-08-15
AU5875286A (en) 1987-03-12

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