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
  • C23C22/46—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 oxalates
• • 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
  • C23C22/07—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 phosphates
  • C23C22/08—Orthophosphates
  • C23C22/10—Orthophosphates containing oxidants
• • 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
  • C23C22/73—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 characterised by the process
• • 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
  • C23C22/78—Pretreatment of the material to be coated
  • C23C22/80—Pretreatment of the material to be coated with solutions containing titanium or zirconium compounds
• • 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
  • C23C22/83—Chemical after-treatment
• • 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

• Such conversion coatings/conversion layers are addi tionally passivated with a passivation layer by contacting it with a passivation composi tion.
• Such passivation compositions and respective methods are known in the art.
• the passivation composition furthermore modifies the color of the conver sion coating/conversion layer, for example into a bluish or even dark black color. De pending on the application, such a color modification is often very much desired for op tical reasons, in particular in the automotive field.
• WO 97/13888 A1 refers to a non-chromate containing, corrosion-inhibiting coating com position capable of protecting a wide variety of metal surfaces.
• WO 02/49960 A2 refers to specific tripolyphosphates, mixtures thereof, and their use as anti-corrosion agents and as biocides (anti-microbial agents) and, where applicable, as encrustation-inhibiting agents.
• composition for depositing the black-passivation layer on the zinc-iron alloy, the composition comprising (i) one or more than one blackening agent selected from the group consisting of formula (I),
• the present invention also concerns a respective black-passivation composition as fur ther described below in the text as well as a respective use of said one or more than one blackening agent for blackening a zinc-iron alloy.
• a respective black-passivation composition as fur ther described below in the text as well as a respective use of said one or more than one blackening agent for blackening a zinc-iron alloy.
• features described in regard to the method of the present invention in particular features described as being pre ferred, apply likewise to the black-passivation composition of the present invention, most preferably to a black-passivation composition described as being preferred, and apply likewise to the use according to the present invention, most preferably to the use de scribed as being preferred.
• black-passivation layer also denotes a black-conversion layer.
• the black-passivation layer has a darkness value L* of 40 or below, preferably of 33 or below, most preferably of 25 or below, based on the CIELAB color space defini tion.
• the method of the present invention generally applies to a zinc-iron alloy.
• Preferred is a method of the present invention, wherein the zinc-iron alloy is present on the substrate as a layer, preferably as a layer resulting from a galvanization process, most preferably from a zinc-iron galvanization process.
• the zinc-iron alloy is distinct from the rest of the substrate. In such a way, the substrate is typically protected from corrosion.
• the substrate comprises iron.
• the substrate preferably comprises a base material, preferably a ferrous base material, more preferably steel, on which the zinc-iron alloy is deposited.
• the zinc-iron alloy is distinct from the rest of the substrate (i.e. is represented by the base material).
• the substrate comprises the zinc-iron alloy in a sense that the substrate itself is made of a zinc-iron alloy.
• the base material is already the zinc-iron alloy and thus, the base material is the substrate.
• the substrate is a metal or metal alloy substrate, preferably the substrate comprises iron, most preferably the substrate comprises iron and is different from the zinc-iron alloy.
• the black-passivation composi tion is acidic, preferably having a pH from 1.0 to 4.5, preferably from 1.2 to 4.0, more preferably from 1.4 to 3.3, even more preferably from 1.5 to 2.8, most preferably from 1.6 to 2.2.
• the one or more than one blackening agent has a total concentration ranging from 0.2 mmol/L to 100 mmol/L, based on the total volume of the black-passivation composi tion, preferably from 0.3 mmol/L to 80 mmol/L, more preferably from 0.4 mmol/L to 60 mmol/L, even more preferably from 0.8 mmol/L to 45 mmol/L, most preferably from 1.6 mmol/L to 38 mmol/L.
• R 3 and R 4 are inde pendently selected from the group consisting of ammonium salts and alkaline salts, pref erably from the group consisting of ammonium, sodium, and potassium.
• n 2, 3, or 4, preferably 3.
• Sulfonic acid preferably means -SChH, wherein denotes the covalent bond connect ing this group with the rest of the compound of formula (I).
• Carboxylic acid preferably means -COOH, wherein denotes the covalent bond connecting this group with the rest of the compound of formula (I).
• R 4 comprises at least sulfonic acid, salts and/or esters thereof, preferably R 4 comprises at least sulfonic acid, salts and/or esters thereof, and m is 3.
• the black-passivation composition utilized in the method of the present invention com prises one or more than one species of metal ions selected from the group consisting of trivalent chromium, titanium, and zirconium.
• metal ions selected from the group consisting of trivalent chromium, titanium, and zirconium.
• a very preferred trivalent chromium ion source is an organic and/or inorganic trivalent chromium ion source.
• a preferred organic trivalent chromium ion source is trivalent chromium citrate.
• a preferred inorganic trivalent chromium ion source is trivalent chromium chloride hexahydrate.
• the metal ions of trivalent chromium have a total concentration ranging from 0.1 g/L to 8.0 g/L, based on the total volume of the black-passivation composition, pref erably from 0.2 g/L to 7.1 g/L, more preferably from 0.5 g/L to 6.1 g/L, even more prefer ably from 0.8 g/L to 5.0 g/L, most preferably from 1.0 g/L to 3.5 g/L.
• the above mentioned total concentration for metal ions of trivalent chromium applies with the proviso that these ions are the only species of transition metal ions in the black-pas sivation composition.
• iron ions are present in a total concentration of 1 g/L or below, based on the total volume of the black-passivation composition, preferably of 0.8 g/L or below, most pref erably of 0.5 g/L or below, after step (C) is carried out multiple times.
• the black-passivation com position is substantially free of, preferably does not comprise, tungsten.
• Said one or more than one carboxylic acid and/or salts thereof typically serve as com plexing agents for said one or more than one species of metal ions selected from the group consisting of trivalent chromium, titanium, and zirconium, most preferably for metal ions of trivalent chromium.
• a preferred dicarboxylic acid and/or salts thereof comprises a C2 to C6 dicarboxylic acid and/or salts thereof, preferably oxalic acid, malonic acid, and/or salts thereof, most pref erably oxalic acid and/or salts thereof.
• a preferred tricarboxylic acid and/or salts thereof comprises citric acid and/or salts thereof.
• the one or more than one car boxylic acid and salts thereof have a total concentration from 0.5 mmol/L to 120 mmol/L, based on the total volume of the black-passivation composition, preferably from 8 mmol/L to 105 mmol/L, even more preferably from 15 mmol/L to 90 mmol/L, most preferably from 30 mmol/L to 80 mmol/L, even most preferably from 45 mmol/L to 70 mmol/L. More pref erably, the above total concentration applies with the proviso that the black-passivation composition comprises at least one or more than one dicarboxylic acid and/or salts thereof.
• the oxalic acid and salts thereof have a total concentration from 0.5 mmol/L to 120 mmol/L, based on the total volume of the black-passivation composi tion, preferably from 8 mmol/L to 105 mmol/L, even more preferably from 15 mmol/L to 90 mmol/L, most preferably from 30 mmol/L to 80 mmol/L, even most preferably from 45 mmol/L to 70 mmol/L.
• oxalic acid and salts thereof are the only dicar- boxylic acids and salts thereof in the black-passivation composition, preferably the only carboxylic acids and salts thereof in the black-passivation composition.
• the black-pas sivation composition comprises citric acid and/or salts thereof, preferably in a total con centration from 0.5 mmol/L to 120 mmol/L, based on the total volume of the black-pas sivation composition, preferably from 8 mmol/L to 105 mmol/L, even more preferably from 15 mmol/L to 90 mmol/L, most preferably from 30 mmol/L to 80 mmol/L, even most preferably from 45 mmol/L to 70 mmol/L.
• citric acid and salts thereof are preferably the only tricarboxylic acid and salts thereof in the black-passivation composi tion, most preferably the only carboxylic acid and salts thereof in the black-passivation composition.
• Nitrate ions preferably act as oxidizing agent in the black-passivation composition.
• the nitrate ions have a total con centration ranging from 0.1 g/L to 20 g/L, based on the total volume of the black-pas sivation composition, preferably from 0.4 g/L to 15 g/L, even more preferably from 0.8 g/L to 11 g/L, most preferably from 1.2 g/L to 7 g/L, even most preferably from 1.7 g/L to 4.5 g/L.
• step (c) the substrate is contacted with the black-passivation composition, preferably as described above, more preferably as described above as being preferred.
• step (c) the black-passivation composition has a temperature in a range from 10°C to 80°C, preferably from 15°C to 65°C, even more preferably from 19°C to 45°C, most preferably from 22°C to 38°C. If the temperature is significantly exceeding 80°C, in many cases an undesired rapid dis solution (stripping) of the zinc-iron alloy is observed impairing the corrosion resistance. However, if the temperature is too low, in many cases the contacting in step (c) is unde sirably long.
• step (c) the contacting is per formed for a time period from 10 seconds to 200 seconds, preferably from 20 seconds to 160 seconds, even more preferably from 40 seconds to 130 seconds, most preferably from 60 seconds to 100 seconds. If the time period is significantly exceeding 200 sec onds, in many cases an undesired rapid dissolution (stripping) of the zinc-iron alloy is observed impairing the corrosion resistance. However, if the time period is too low, typi cally the blackening is insufficient and thus, the optical appearance is negatively im paired.
• step (c) is performed without applying an electrical current.
• the substrate is dipped into the black-passivation composition.
• step (c) an indeed very good corrosion resistance is obtained if after step (c) the substrate is further treated in order to increase corrosion resistance.
• step (c) of the method of the present invention is additionally treated with a post-dip composition and/or a sealer composition, preferably as outlined below, either in this order or in reversed order.
• step (c) is followed by step
• step (d) contacting the substrate obtained after step (c) with a post-dip composition such that a post-dipped substrate is obtained.
• the post-dip composition is acidic, preferably has a pH ranging from 3.0 to 6.8, more preferably from 3.5 to 6.5, even more preferably from 4.0 to 6.3, most preferably from 4.3 to 6.0.
• step (d) the post-dip compo sition has a temperature in a range from 18°C to 60°C, preferably 20°C to 58°C, more preferably from 28°C to 56°C, even more preferably from 33°C to 54°C, most preferably from 38°C to 50°C.
• step (d) is a method of the present invention, wherein in step (d) the contacting is per formed for a time period from 5 seconds to 200 seconds, preferably from 10 seconds to 140 seconds, even more preferably from 20 seconds to 100 seconds, most preferably from 30 seconds to 70 seconds.
• step (d) is followed by step
• step (e) contacting the substrate obtained after step (d) with a sealer composition such that a sealed substrate is obtained.
• the sealer composition is alka line, preferably has a pH of 9 or higher, more preferably in a range from 9.1 to 12, even more preferably from 9.3 to 11 , most preferably from 9.5 to 10.5.
• sealer composition comprises two or more than two organic compounds.
• sealer composition comprises one or more than one wax.
• the sealer composition comprises one or more than one silicon-containing compound, preferably at least one silane and/or at least one inorganic silicate.
• the at least one inorganic silicate is a colloid.
• step (e) the sealer composition has a temperature in a range from 15°C to 35°C, preferably 17°C to 30°C, more prefer ably from 19°C to 27°C, most preferably from 21 °C to 25°C.
• step (e) is a method of the present invention, wherein in step (e) the contacting is per formed for a time period from 5 seconds to 200 seconds, preferably from 10 seconds to 140 seconds, even more preferably from 20 seconds to 100 seconds, most preferably from 30 seconds to 70 seconds.
• step (f) is carried out at a tem perature ranging from 55°C to 95°C, preferably 58°C to 90°C, more preferably from 58°C to 85°C, most preferably from 60°C to 80°C.
• step (f) is carried out for a time period from 2 minutes to 20 minutes, preferably from 3 minutes to 16 minutes, even more preferably from 4 minutes to 13 minutes, most preferably from 6 minutes to 10 minutes.
• a drying step is also carried out after one or more than one of the previous steps, e.g. after step (c), step (d), etc.
• a drying step preferably as defined in step (f) is carried out after step (d) and prior to step (e). This is very preferred because in step (d) the post-dip composition is acidic, wherein in step (e) the sealer composition is alka line.
• the present invention furthermore refers to a black-passivation composition for deposit ing a black-passivation layer on a zinc-iron alloy, the composition comprising
• R 1 and R 2 are independently selected from the group consisting of hydro gen and C1 to C5 alkyl
• the black-passivation composition is substantially free of, preferably does not comprise, nickel ions, cobalt ions, and tungsten ions.
• the aforementioned regarding the black-passivation composition utilized in the method of the present invention applies likewise to the black-passivation composition of the present invention.
• the present invention furthermore refers to the use of one or more than one blackening agent selected from the group consisting of formula (I),
• R 3 is selected from the group consisting of sulfonic acid, carboxylic acid, alkyl carboxylic acid, phosphonic acid, salts and esters thereof, and n is 1 , 2, 3, 4, or 5, and formula (II), wherein
• test passivation compositions were prepared with the number ing as introduced in Table 1 below, each composition is aqueous and generally com prises a species of metal ions; 6 g/L to 8 g/L chloride ions if chromium ions were utilized; 50 mmol/L to 70 mmol/L oxalic acid if chromium ions were utilized or 10 mmol/L to 300 mmol/L fluoride ions if titanium ions and zirconium ions were utilized, respectively, as complexing agents; approximately 1 g/L to 7 g/L nitrate ions; and one of the following compounds abbreviated as below:
• DPS 3-(N,N-Dimethylthiocarbamoyl)-thiopropanesulfonate, sodium salt; also known as Raluplate DPS (CAS 18880-36-9; Raschig company); a compound of formula (I), wherein R 1 and R 2 are methyl, R 3 is the sodium salt of sulfonic acid, and n is 3;
• ZPS 3-(2-Benzthiazolylthio)-1-propanesulfonate, sodium salt; also known as Raluplate ZPS (CAS 49625-94-7; Raschig company); a compound of formula (II), wherein R 4 is the sodium salt of sulfonic acid, and m is 3;
• SPV 1-(3-Sulfopropyl)-2-vinylpyridinium betaine; also known as Raluplate SPV (CAS 90552-35-5; Raschig company); comparative example;
• MPS 3-Mercaptopropanesulfonate, sodium salt; also known as Raluplate MPS (CAS 17636-10-1; Raschig company); comparative example;
• test passivation composition has a pH of approximately 2.
• a plurality of u-shaped iron plate specimens base ma terial galvanized with a silver-like colored zinc-iron layer (Hiron-Zn/Fe for high iron con tent and Protedur Plus for low iron content, respectively, each is a product of Atotech; for iron content see Table 1 below) was dipped for approximately 90 seconds in the respective test passivation composition, the compositions having a temperature of ap proximately 22°C. In examples according to the invention, a blackening was immediately observed.
• test passivation compositions in particular ac cording to the present invention
• ac cording to the present invention were tested with said substrates but having a zinc (no zinc alloy) or a zinc-nickel alloy layer thereon.
• no blackening was obtained (i.e. evaluated as “-“).
• the test passivation compositions utilized in the method of the present invention very specifically blacken zinc-iron alloys.

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