WO2008144140A1 - Bain de conditionneur de rinçage pour traiter un substrat et procédé associé - Google Patents

Bain de conditionneur de rinçage pour traiter un substrat et procédé associé Download PDF

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Publication number
WO2008144140A1
WO2008144140A1 PCT/US2008/060547 US2008060547W WO2008144140A1 WO 2008144140 A1 WO2008144140 A1 WO 2008144140A1 US 2008060547 W US2008060547 W US 2008060547W WO 2008144140 A1 WO2008144140 A1 WO 2008144140A1
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WO
WIPO (PCT)
Prior art keywords
rinse conditioner
bath
salt
conditioner bath
iron
Prior art date
Application number
PCT/US2008/060547
Other languages
English (en)
Inventor
Jeffrey Allen Green
Donald R. Vonk
Michel Sudour
Mark W. Simpson
Original Assignee
Ppg Industries Ohio, Inc.
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 Ppg Industries Ohio, Inc. filed Critical Ppg Industries Ohio, Inc.
Publication of WO2008144140A1 publication Critical patent/WO2008144140A1/fr

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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
    • C23C22/78—Pretreatment of the material to be coated
    • C23C22/80—Pretreatment of the material to be coated with solutions containing titanium or zirconium compounds

Definitions

  • This invention relates to a rinse conditioner bath comprising a Jernstedt salt and a soluble iron and a method for using the same.
  • Phosphate conversion coatings are well known for treating metal surfaces, particularly ferrous, zinc and aluminum metals and their alloys. When applied, these phosphate coatings form a phosphate layer, primarily of zinc and iron phosphate crystals, which provides corrosion resistance and/or enhances the adhesion of subsequently applied coatings.
  • the metal substrate Prior to application of the phosphate coating, the metal substrate is typically "conditioned” or “activated” by subjecting the surface of the metal substrate to a diluted aqueous dispersion, sometimes referred to as a rinse conditioner bath or activator, by introducing or immersing the metal substrate into a tank that contains the rinse conditioner bath. "Activation" of the surface of the metal substrate is achieved due to the adsorption of colloidal titanium-phosphate particles, which are present in the rinse conditioner bath, to the metal's surface.
  • colloidal titanium- phosphate particles have a tendency to agglomerate in the rinse conditioner bath due to dissolved calcium (Ca 2+ ) and magnesium (Mg 2+ ) ions (hard water ions) that are typically present in the rinse conditioner bath.
  • the hard water ions are usually introduced into the rinse conditioner bath via the water that is used to create the rinse conditioner bath. Accordingly, to prevent agglomeration of the colloidal titanium-phosphate particles, chelating or sequestering compounds, such as polyphosphates and pyrophosphates, are introduced into the rinse conditioner bath.
  • the present invention is directed to a rinse conditioner bath comprising a
  • the present invention is also directed to a method for treating a substrate comprising applying a rinse conditioner bath comprising a Jernstedt salt and a soluble iron to at least a portion of the substrate, and phosphatizing at least a portion of the substrate with an aqueous zinc phosphate solution.
  • the present invention is further directed to a rinse conditioner concentrate comprising a Jernstedt salt and another salt, wherein the another salt comprises a soluble iron.
  • FIG. 1 is a top elevation view of a surface of a cold-rolled steel panel under a scanning electron microscope at 100Ox after the cold-rolled steel panel has been phosphatized with a zinc phosphate solution;
  • FIG. 2 is a top elevation view of a surface of another cold-rolled steel panel under a scanning electron microscope at 1000x after the cold-rolled steel panel has been phosphatized with a zinc phosphate solution;
  • FIG. 3 is a top elevation view of a surface of yet another cold-rolled steel panel under a scanning electron microscope at 1000x after the cold-rolled steel panel has been phosphatized with a zinc phosphate solution;
  • FIG. 4 is a top elevation view of a surface of yet another cold-rolled steel panel under a scanning electron microscope at 1000x after the cold-rolled steel panel has been phosphatized with a zinc phosphate solution.
  • the phrase "rinse conditioner bath” will refer to an aqueous solution and/or a colloidal suspension that is applied onto at least a portion of a substrate and/or into which at least a portion of a substrate is immersed in order to promote the formation of a zinc phosphate coating on at least a portion of the substrate that was treated with the rinse conditioner bath. It is, therefore, understood that the substrate is treated with the rinse conditioner bath prior to phosphatizing at least a portion of the treated substrate with a zinc phosphate solution.
  • the phrase "soluble iron” refers to an iron compound that is soluble in an aqueous medium such as water or a solvent.
  • the "soluble iron” is ferrous iron (i.e., Fe 2+ ) that is formed by dissociation of a salt in an aqueous medium.
  • the "soluble iron” is ferrous iron that is a reaction product of ferric iron (i.e., Fe 3+ , Fe(III)) and a reducing agent such as, without limitation, hydrogen peroxide (H 2 O 2 ), which is produced in situ.
  • a reducing agent such as, without limitation, hydrogen peroxide (H 2 O 2 ), which is produced in situ.
  • H 2 O 2 hydrogen peroxide
  • the present invention is directed to a rinse conditioner bath that is utilized to "activate” or “condition” at least a portion of a substrate prior to phosphatizing at least a portion of a substrate with a zinc phosphate solution.
  • the rinse conditioner bath promotes the formation of zinc and zinc/iron phosphate crystals on the substrate when at least a portion of the substrate, which was subjected to the rinse conditioner bath, is phosphatized with a zinc phosphate solution.
  • a suitable substrate that can be treated with the rinse conditioner include, but are not limited to, a metal and/or a metal alloy.
  • the metal and/or metal alloy can be aluminum, steel, or zinc.
  • a steel substrate could include cold rolled steel, electrogalvanized steel, and hot dipped galvanized steel.
  • the substrate may comprise a portion of a vehicle such as a vehicular body (e.g., without limitation, door, body panel, trunk deck lid, roof panel, hood, and/or roof) and/or a vehicular frame.
  • the rinse conditioner bath is comprised of a Jernstedt salt and a soluble iron.
  • the Jernstedt salt typically comprises titanium-phosphate particles such as colloidal titanium-phosphate particles.
  • the Jernstedt salt is Na 4 TiO(PO 4 ) 2 .
  • the addition of soluble iron to the rinse conditioner bath dramatically increases the "life span" of the rinse conditioner bath.
  • life span will refer to the total amount of time (e.g., hours, days, weeks, months, etc ..) that the rinse conditioner bath is capable of promoting the formation of zinc phosphate on a substrate. Accordingly, it will be understood that an increase in the "life span" of the rinse conditioner bath will mean that the rinse conditioner bath will not have to be replaced as often, when compared to a rinse conditioner bath that lacks soluble iron, since the rinse conditioner bath disclosed in this invention is capable of promoting the formation of zinc phosphate on the substrate over an extended period of time.
  • the soluble iron is introduced into a rinse conditioner bath via a salt such as, without limitation, ferrous nitrate, ferrous sulfate, ferrous chloride, ferrous gluconate, or combinations thereof.
  • the salt can either be in solid form (e.g. powder/particulate form) or in aqueous form (i.e., dissociated ions in an aqueous medium).
  • an aqueous rinse conditioner concentrate which comprises the salt in aqueous form, a liquid thickener, chelating compound(s), and a Jernstedt salt, is added to an aqueous solution, such as water, to form the disclosed rinse conditioner bath.
  • Suitable liquid thickeners that can be used in the aqueous rinse conditioner concentrate would include, but are not limited to, hydroxyl methyl cellulose, xanthan gum, and polycarboxylic acid, and combinations thereof.
  • the rinse conditioner is formed by the introduction of a powder concentrate, which comprises a chelating compound, into an aqueous solution, such as water, to form a precursor to the rinse conditioner bath.
  • the salt which is in aqueous and/or solid form, is then added to the precursor to the rinse conditioner bath in order to form the disclosed rinse conditioner bath.
  • the salt, which is in solid form is added to a powder concentrate before the powder concentrate is added to the aqueous solution to form the disclosed rinse conditioner.
  • the aqueous rinse conditioner concentrate as well as the powder concentrate will be collectively referred to as a rinse conditioner concentrate.
  • the rinse conditioner concentrate is typically used to make the rinse conditioner bath that is applied onto a substrate prior to the substrate being subjected to a phosphatizing step using a zinc phosphate solution.
  • the aqueous solution to which the rinse conditioner concentrate is added could be an aqueous solution which has low hardness.
  • the phrase "low hardness" refers to an aqueous solution containing ⁇ 25 ppm of calcium carbonate and/or magnesium.
  • the aqueous solution could be deionized water, distilled water, reverse osmosis water, or combinations thereof.
  • the soluble iron can be present in the rinse conditioner bath in an amount ranging from 5 to 1000 ppm based on the total weight of the rinse conditioner bath. In another embodiment, the soluble iron can be present in the rinse conditioner bath in an amount ranging from 20 to 30 ppm based on the total weight of the rinse conditioner bath. As demonstrated in the examples below, addition of soluble iron into the rinse conditioner bath can increase the "life span" of the rinse conditioner bath.
  • the addition of soluble iron into the rinse conditioner bath extends the "life span" of the rinse conditioner bath because the chelating/sequestering compounds, which are typically added to the rinse conditioner bath, have a preference to attack the soluble iron as opposed to attacking and causing the dissolution of the Jernstedt salt. Because the Jernstedt salt is not dissolved by the chelating/sequestering compounds, the Jernstedt salt would continue to promote the formation of zinc and iron phosphate crystals on the substrate that is being treated.
  • the rinse conditioner bath to which the soluble iron is added comprises sodium phosphate, potassium phosphate, and titanium wherein the titanium is present as a complex salt with either or both sodium phosphate and the potassium phosphate.
  • Suitable sodium phosphates useful in the rinse conditioner bath described in the preceding paragraph include, without limitation, mono- di- or tri-sodium phosphate, pentasodium triphosphate (also known as sodium tripolyphosphate), tetrasodium diphosphate,(tetrasodium pyrophosphate) disodium orthophosphate, pentasodium triphosphate, or combinations thereof.
  • Suitable potassium phosphates useful in the rinse conditioner bath include, without limitation, mono-, di- or tri- potassium phosphate, pentapotassium triphosphate (also known as potassium tripolyphosphate), dipotassium orthophosphate, tetrapotassium pyrophosphate or combinations thereof.
  • a variety of titanium (IV) compounds or salts may be used as the source of titanium in the rinse conditioner bath as long as the anion of the salt does not interfere with the subsequent zinc phosphate pretreatment.
  • titanium halides, titanium oxides (e.g., titanium dioxide), titanium sulfates and titanium oxalates may be used. While the selection of the titanium source is not limited, titanium halides, specifically potassium titanium fluoride is most suitable.
  • the rinse conditioner bath may further comprise additional optional components such as, without limitation, diphosphonic acids, alkali metal carbonates or hydroxides and/or thickening agents ⁇ e.g., xanthans, polysaccharides and polycarboxylates).
  • additional optional components such as, without limitation, diphosphonic acids, alkali metal carbonates or hydroxides and/or thickening agents ⁇ e.g., xanthans, polysaccharides and polycarboxylates).
  • the rinse conditioner bath described above can be prepared by introducing a rinse conditioner concentrate to an aqueous medium such as water.
  • the rinse conditioner concentrate is prepared by mixing in an aqueous medium a sodium phosphate with a titanium compound and heating the mixture to form a paste-like pre-mix.
  • the paste-like premix can be made by adding pentasodium triphosphate to water, which is preheated to a temperature ranging from 65 0 C to 95 0 C, in order to form a slurry.
  • a titanium compound is then added to the slurry and the slurry is agitated.
  • disodium orthophosphate is added to the slurry and the slurry mixed thoroughly for about 5 to 15 minutes.
  • a paste-like pre-mix containing the titanium phosphate complex salt is produced.
  • the paste-like pre-mix is then combined with potassium phosphate and other ingredients, such as a liquid thickener, to form the conditioner concentrate.
  • the potassium phosphate may be one or a combination of the potassium phosphates described above. It is generally suitable to use dipotassium orthophosphate or a combination of dipotassium orthophosphate and pentapotassium triphosphate, tetrapotassium pyrophosphate is additionally suitable when activating aluminum substrates. It is noted that in other embodiment, the paste-like pre-mix may be added to the potassium phosphate hot or after a cooling period.
  • the rinse conditioner concentrate is a concentrated aqueous dispersion of a titanium containing phosphate composition.
  • the sodium phosphate is present in amounts of from 10% to 30% by weight
  • the potassium phosphate is present in amounts of from 20% to 40% by weight
  • the titanium is present in amounts of from 0.05% to 2.5% by weight
  • water is present in amounts of from 30% to 60% by weight, the percentage by weight based on the total weight of the ingredients used in making the rinse conditioner concentrate.
  • the sodium phosphate is disodium orthophosphate in combination with pentasodium triphosphate, and the disodium orthophosphate is present in amounts of from 10% to 25% by weight and the pentasodium triphosphate is present in amounts of from 1 % to 10% by weight, the percentage by weight being based on total weight of ingredients used in making the rinse conditioner concentrate.
  • the potassium phosphate is preferably dipotassium orthophosphate in combination with pentapotassium triphosphate, and the dipotassium orthophosphate is typically present in amounts of from 5% to 20% by weight and the pentapotassium triphosphate is present in amounts of from 10% to 25% by weight, the percentage by weight being based on total weight of ingredients used in making the rinse conditioner concentrate.
  • the tetrapotassium pyrophosphate is present in amounts of up to 5% by weight based on total weight of the ingredients used in the making of the rinse conditioner concentrate.
  • a substrate is treated by (a) applying a rinse conditioner bath comprising a Jernstedt salt and a soluble iron to a least a portion of the substrate, and (b) phosphatizing at least a portion the substrate with an aqueous zinc phosphate solution.
  • the rinse conditioner bath can be applied to the substrate by spray, roll-coating or immersion techniques.
  • the rinse conditioner bath is typically applied onto the substrate at a temperature ranging from 2O 0 C to 5O 0 C for any suitable period of time.
  • the surface of the substrate is subjected to a phosphate pretreatment such as a zinc phosphate pretreatment.
  • the phosphatizing step can be performed by spray application or immersion of the activated substrate in an acidic phosphate bath which contains zinc and other divalent metals known in the art at a temperature ranging from 35 0 C to 75 0 C for 1 to 3 minutes.
  • the substrate is optionally post-rinsed with a chromium or non-chromium containing solution, rinsed with water and optionally dried. Paint is then typically applied, such as, by electrodeposition or by conventional spray or roll coating techniques.
  • the present invention is also directed to a conditioner stage such as those used in an automotive manufacturing facility.
  • the conditioner stage comprises an immersion tank which contains the rinse conditioner bath that is disclosed in this invention.
  • the rinse conditioner bath is contained within the immersion tank at a temperature ranging from 2O 0 C to 5O 0 C.
  • a portion of the substrate is subjected to the rinse conditioner bath by immersing the substrate in the rinse conditioner bath for any suitable period of time.
  • a portion of the "activated" substrate is then subjected to a phosphatizing step by applying a zinc phosphate solution to the "activated" substrate.
  • additional rinse conditioner bath can be sprayed onto a portion of the "activated” substrate via a spraying nozzle as the "activated" substrate is removed from the immersion tank.
  • the spraying nozzle could be an "exit halo" which is positioned downstream from the immersion tank.
  • the conditioner stage comprises a number of spraying nozzles that are used to apply the rinse conditioner bath onto a least a portion of a substrate.
  • a spray tank Disposed beneath the spraying nozzles is a spray tank which is adapted to collect the rinse conditioner bath that exits the spraying nozzles and/or any excess rinse conditioner bath that drips off the surface of the "activated" substrate.
  • the spray tank is connected to the spraying nozzles in a manner that allows the spraying nozzles to utilize the rinse conditioner bath that is collected in the spray tank thereby recycling the rinse conditioner bath.
  • the "activated" substrate is then phosphatized as described in the preceding paragraph.
  • Two 4 liter rinse conditioner baths Baths A and B, were prepared by adding 1 .0 gram of a commercially available Liquid Rinse Conditioner (available from PPG Industries, Inc. of Pittsburgh, PA) per 1 liter of deionized water. No ferrous iron (Fe(II)) was added to Bath A while ferrous iron was added to Bath B at a concentration of 20 ppm (0.4g FeSo 4 .7H 2 0). It will be understood that Bath A is the control.
  • Liquid Rinse Conditioner available from PPG Industries, Inc. of Pittsburgh, PA
  • FIG. 1 this is a top elevation view of the surface 2 of Steel Panel D after Steel Panel D was phosphatized with CHEMFOS 700AL.
  • the extensive number of nodular crystalline structures 4 seen in FIG. 1 is the zinc phosphate coating 6 that was formed over essentially the entire surface 2 of Steel Panel D during the phosphatizing process.
  • the formation of the substantially uniform zinc phosphate coating on the surface of Steel Panel D was promoted by the rinse conditioner bath of Bath A. Accordingly, the rinse conditioner bath of Bath A was active.
  • the term “active” will refer to a rinse conditioner bath's ability to promote the formation a zinc phosphate coating on a substrate.
  • FIG. 2 this is a top elevation view of the surface 8 of Steel Panel E after Steel Panel E was phosphatized with CHEMFOS 700AL. Similar to the zinc phosphate coating that is seen in FIG. 1 , the extensive number of nodular crystalline structures 10 seen in this figure is a substantially uniform zinc phosphate coating 12 that was formed over essentially the entire surface 8 of Steel Panel E during the phosphatizing process. The formation of the extensive zinc phosphate coating 12 on the surface 8 of Steel Panel E was promoted by the rinse conditioner bath of Bath B. In other words, the rinse conditioner in Bath B, like Bath A, was active.
  • Bath B the rinse conditioner in Bath B, like Bath A
  • FIG. 4 this is a top elevation view of the surface 18 of Steel Panel Z after Steel Panel Z was phosphatized with CHEMFOS 700AL.
  • Steel Panel Z contained an extensive number of nodular crystalline structures similar to those observed in Steel Panels D and E.
  • the formation of the nodular crystalline structures 20 (i.e., the zinc phosphate coating) on the surface 18 of Steel Panel Z was promoted by the rinse conditioner bath of Bath B.
  • the rinse conditioner bath of Bath B was active, even after 24 hours, due to the addition of ferrous iron to the rinse conditioner bath of Bath B.

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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)

Abstract

L'invention concerne un bain de conditionneur de rinçage qui comporte un sel de Jernstedt et un fer soluble. Un procédé pour traiter un substrat avec le bain de conditionneur de rinçage décrit ainsi qu'une solution de phosphate de zinc sont également proposés.
PCT/US2008/060547 2007-05-17 2008-04-17 Bain de conditionneur de rinçage pour traiter un substrat et procédé associé WO2008144140A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US11/749,906 2007-05-17
US11/749,906 US20080283152A1 (en) 2007-05-17 2007-05-17 Rinse conditioner bath for treating a substrate and associated method

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WO2008144140A1 true WO2008144140A1 (fr) 2008-11-27

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Publication number Priority date Publication date Assignee Title
DE102013202286B3 (de) * 2013-02-13 2014-01-30 Chemetall Gmbh Verwendung eines Silan-, Silanol- oder/und Siloxan-Zusatzes zur Vermeidung von Stippen auf Zink-haltigen Metalloberflächen und Verwendung der beschichteten Metallsubstrate
RU2729485C1 (ru) 2016-08-24 2020-08-07 Ппг Индастриз Огайо, Инк. Железосодержащая композиция очистителя

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US4152176A (en) * 1978-08-07 1979-05-01 R. O. Hull & Company, Inc. Method of preparing titanium-containing phosphate conditioner for metal surfaces
BE894432A (fr) * 1981-09-17 1983-01-17 Amchem Prod Solutions d'enduction aqueuses, acides, de phosphate de zinc, concentrats pour les constituer, solutions d'activation et procedes pour leur mise en oeuvre
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US20060060265A1 (en) * 2004-09-21 2006-03-23 Henkel Kommanditgesellschaft Auf Aktien Lubricant system for cold forming, process and composition therefor

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