EP0454211B1 - Procédé pour appliquer des couches de phosphates sur des surfaces métalliques - Google Patents

Procédé pour appliquer des couches de phosphates sur des surfaces métalliques Download PDF

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Publication number
EP0454211B1
EP0454211B1 EP91200844A EP91200844A EP0454211B1 EP 0454211 B1 EP0454211 B1 EP 0454211B1 EP 91200844 A EP91200844 A EP 91200844A EP 91200844 A EP91200844 A EP 91200844A EP 0454211 B1 EP0454211 B1 EP 0454211B1
Authority
EP
European Patent Office
Prior art keywords
activating
phosphate
copper
steel
quantities
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
EP91200844A
Other languages
German (de)
English (en)
Other versions
EP0454211A1 (fr
Inventor
Rüdiger Rein
Dieter Dr. Jentsch
Klaus-Werner Dr. Wittel
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
Continentale Parker SA
Original Assignee
Metallgesellschaft AG
Continentale Parker SA
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, Continentale Parker SA filed Critical Metallgesellschaft AG
Publication of EP0454211A1 publication Critical patent/EP0454211A1/fr
Application granted granted Critical
Publication of EP0454211B1 publication Critical patent/EP0454211B1/fr
Anticipated expiration legal-status Critical
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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

  • the invention relates to a method for applying phosphate coatings on metal surfaces by activation with an activating agent based on Ti IV phosphate and zinc phosphating.
  • zinc phosphate layers can be produced on numerous metallic surfaces, such as iron, steel, galvanized alloy steel, aluminum or aluminized steel.
  • the zinc phosphate layers obtained serve to protect against corrosion, paint adhesion, reduction of sliding resistance, ease of cold forming and electrical insulation.
  • a phosphating process also includes various pre-treatment and post-treatment stages. It is essential to clean the metal surface, which is generally done with alkaline or acidic cleaners and removes oils, greases, oxides and adhering solid particles from the metal surface. If cleaning is carried out with mildly alkaline cleaners, it is in principle possible to combine cleaning with activation of the metal surface. As a rule, however, the activation follows the cleaning as a separate process step.
  • the task of activating the metal surface is to form a with the shortest possible phosphating times to ensure the finest possible crystalline zinc phosphate layer.
  • a criterion for the effectiveness of an activating agent is therefore the minimum phosphating time.
  • the suitability for forming even finely crystalline zinc phosphate layers can be determined on the basis of the layer weights or by scanning electron microscope images.
  • Titan IV phosphates form when aqueous titanium IV salt solutions are reacted with soluble phosphates or phosphoric acid.
  • products with activating properties are only obtained under special manufacturing conditions, which are described, for example, in US Pat. Nos. 2,310,239 and 2,456,947 and provide precise information regarding the type and concentration of the raw materials, temperature and pH range during manufacture.
  • the reaction conditions are kept constant, there are fluctuations in the application effect from batch to batch.
  • activation agents based on titanium IV phosphate have to be prepared with deionized water.
  • the reason for this is that the alkaline earth metal ions present in the tap water as hardening agents destabilize titanium IV phosphate in activation baths.
  • These alkaline earth metal ions can also be introduced into the activation bath by rinsing water.
  • DE-A-3731089 proposes that cation-exchanging zeolites with a primary particle diameter of ⁇ 3 »m the activating one Mix in titanium phosphate.
  • Another way to improve the activation baths is described in EP-B-180523.
  • the addition of phosphonic acid acting as a complexing agent into the activation bath permits the use of industrial water for the bath preparation.
  • the phosphonic acid is said to cause the zinc phosphate layer to become extremely fine crystalline.
  • a serious disadvantage of individual phosphonic acids is that they act as a phosphating bath poison even in concentrations of a few mg / l. An entry of phosphonic acid from the activation bath into the phosphating bath can render the phosphating bath unusable in a very short time.
  • DE-A-3814287 provides for poly (aldehyde carboxylic acids) to be added in substoichiometric amounts as complexing agents for titanium IV during the production of activating titanium IV phosphates.
  • the introduction of the poly (aldehyde carboxylic acids) into the phosphating bath can have considerable disadvantages.
  • Activating agents based on Ti IV phosphate containing at least one of the divalent metals barium, strontium and calcium are also known (FR-A-2 114 874).
  • the number of equivalents of titanium should not exceed the number of equivalents of divalent metals.
  • the result of the activating cleaning prior to zinc phosphating is reported using cleaning liquids which have a pH greater than 12 and which contain, inter alia, an activating agent based on Ti IV phosphate modified with a copper compound. According to the presentation in FR-A-2 114 874, this pretreatment leads to thin, powdery, irregular phosphate layers with coarse crystals in the subsequent zinc phosphating.
  • the object of the invention is to provide a method for applying phosphate coatings on metal surfaces by activation with an activating agent based on Ti IV phosphate and zinc phosphating, which does not have the disadvantages of the known processes, provides for the use of an activating agent which is simple to produce and for stable activation baths with a long service life, which also guarantee the formation of fine crystalline zinc phosphate layers in a short time.
  • 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 activated with an activation bath which 0.001 to 0.060 g / l Ti 0.020 to 1.2 g / l orthophosphate (calc. As P2O5) and 0.001 to 0.1 g / l Cu and contains so much alkali that it has a pH of 7 to 11.
  • an activation bath which 0.001 to 0.060 g / l Ti 0.020 to 1.2 g / l orthophosphate (calc. As P2O5) and 0.001 to 0.1 g / l Cu and contains so much alkali that it has a pH of 7 to 11.
  • the copper content was adjusted by adding copper compounds. These compounds have the effect that the minimum phosphating time is reduced considerably.
  • the addition of copper also means that the activation bath is stable over a wide temperature range and shows very good activating properties.
  • the activating agent contains copper compounds introduced via copper hydroxide, copper oxide hydrate, copper tartrate, copper nitrate and / or copper phosphate. Copper sulfate or copper chloride can be used but are not preferred.
  • Copper concentrations above 0.1 g / l should be avoided since they can lead to a disruption in the phosphating in the subsequent step.
  • activating agent was produced which corresponded to activating agent 2 in terms of composition, but did not contain any copper phosphate.
  • Activating agent 1 was used as activating agent 3, to which maleic anhydride copolymer was added in such a way that the resulting activating bath contained 10 mg / l.
  • Activating agent 1 which was mixed with surfactant in such quantities that the surfactant concentration of 0.3 g / l was formed when the activation bath was prepared, also served as the starting product.
  • the degree of layer coverage was determined in percent. This value indicates the proportion of the metal surface that is provided with a closed zinc phosphate layer.
  • the assessment was made visually.
  • the layer weight of the phosphate coating was determined gravimetrically and the minimum phosphating times determined.
  • the minimum phosphating time is the minimum time required to form a closed phosphate layer.
  • the crystallinity of the phosphate layers was checked using scanning electron microscope images at a magnification of 2000 times.
  • the activating agent according to Examples 1, 2, 3 and 4 leads to a high, almost complete coverage of the metal surface after just 3 minutes of phosphating or enables short treatment times in the subsequent phosphating step.
  • the weight of the phosphate layer is well within the usual range.
  • the results for the activating agents 3 and 4 indicate that the addition of maleic anhydride copolymer or surfactant leads to a considerable increase in the service life of the activating bath if the short minimum phosphating time is observed (cf. activating agent 1).
  • the investigations with the scanning electron microscope showed that the phosphate layers obtained using the activating agents 1, 2, 3 and 4 were of fine-grained nature.

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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)
  • Detergent Compositions (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Materials For Medical Uses (AREA)

Claims (4)

  1. Procédé d'application de revêtements de phosphate sur des surfaces métalliques par activation par un agent d'activation à base de phosphate de Ti IV et par phosphatation au zinc, caractérisé en ce qu'il consiste à activer les surfaces métalliques par un bain d'activation qui contient
    de 0,001 à 0,060 g/l de Ti
    de 0,020 à 1,2 g/l d'orthophosphate (exprimé en P₂O₅)
    de 0,001 à 0,1 g/l de Cu
    et tant d'agent alcalin qu'il ait un pH de 7 à 11.
  2. Procédé suivant la revendication 1, caractérisé en ce qu'il consiste à activer les surfaces métalliques par un bain d'activation qui contient des composés de cuivre introduits par l'intermédiaire de l'hydroxyde de cuivre, de l'hydrate d'oxyde de cuivre, du tartrate de cuivre, du nitrate de cuivre et/ou du phosphate de cuivre.
  3. Procédé suivant la revendication 1 ou 2, caractérisé en ce que le bain d'activation a une teneur supplémentaire en au moins l'un des constituants que sont
    - un phosphate condensé (exprimé en P₂O₅) en des quantités allant jusqu'à 1,2 g/l
    - un silicate (exprimé en SiO₂) en des quantités allant jusqu'à 0,5 g/l
    - un agent complexant en des quantités allant jusqu'à 1,0 g/l
    - un polymère organique hydrosoluble en des quantités allant jusqu'à 0,1 g/l
    - un agent épaississant en des quantités allant jusqu'à 0,1 g/l
    - un agent tensioactif en des quantités allant jusqu'à 0,3 g/l
  4. Utilisation du procédé suivant l'une ou plusieurs des revendications 1 à 3 pour l'activation du fer, de l'acier, de l'acier zingué, de l'acier zingué allié, de l'acier aluminé et de l'aluminium.
EP91200844A 1990-04-21 1991-04-11 Procédé pour appliquer des couches de phosphates sur des surfaces métalliques Expired - Lifetime EP0454211B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4012795 1990-04-21
DE4012795A DE4012795A1 (de) 1990-04-21 1990-04-21 Aktivierungsmittel fuer die phosphatierung

Publications (2)

Publication Number Publication Date
EP0454211A1 EP0454211A1 (fr) 1991-10-30
EP0454211B1 true EP0454211B1 (fr) 1994-06-22

Family

ID=6404842

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91200844A Expired - Lifetime EP0454211B1 (fr) 1990-04-21 1991-04-11 Procédé pour appliquer des couches de phosphates sur des surfaces métalliques

Country Status (9)

Country Link
US (1) US5160551A (fr)
EP (1) EP0454211B1 (fr)
JP (1) JP3063921B2 (fr)
AT (1) ATE107711T1 (fr)
BR (1) BR9101616A (fr)
CA (2) CA2040859C (fr)
DE (2) DE4012795A1 (fr)
ES (1) ES2055518T3 (fr)
ZA (1) ZA912943B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008054407A1 (de) 2008-12-09 2010-06-10 Chemetall Gmbh Verfahren zur Beschichtung von metallischen Oberflächen mit einem Aktivierungsmittel vor dem Phosphatieren
DE102018216216A1 (de) * 2018-09-24 2020-03-26 Thyssenkrupp Ag Verfahren zur Verbesserung der Phosphatierbarkeit von metallischen Oberflächen, welche mit einer temporären Vor- bzw. Nachbehandlung versehen werden
WO2021116318A1 (fr) 2019-12-13 2021-06-17 Thyssenkrupp Steel Europe Ag Procédé de production d'un produit plat en acier ayant une couche de protection métallique à base de zinc et une couche de phosphatation produite sur une surface de la couche de protection métallique, et produit plat en acier de ce type

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2686622B1 (fr) * 1992-01-29 1995-02-24 Francais Prod Ind Cfpi Concentre pour bain d'activation et d'affinage et bain obtenu a partir de ce concentre.
US5628838A (en) * 1992-01-29 1997-05-13 C.F.P.I Societe Anonyme Concentrate for activating and defining bath and bath obtained from this concentrate
DE4232292A1 (de) * 1992-09-28 1994-03-31 Henkel Kgaa Verfahren zum Phosphatieren von verzinkten Stahloberflächen
DE4416619A1 (de) * 1994-05-11 1995-11-16 Henkel Kgaa Herstellung phosphathaltiger Aktiviermittel für die Phosphatierung unter Einsatz von Mikrowellen
US5494504A (en) * 1994-09-12 1996-02-27 Ppg Industries, Inc. Liquid rinse conditioner for phosphate conversion coatings
JP3451334B2 (ja) * 1997-03-07 2003-09-29 日本パーカライジング株式会社 金属のりん酸塩皮膜化成処理前の表面調整用前処理液及び表面調整方法
MY129412A (en) * 1998-07-21 2007-03-30 Nihon Parkerizing Conditioning liquid and conditioning process used in pretreatment for formation of phosphate layer on the metallic surface
JP2007204835A (ja) * 2006-02-03 2007-08-16 Nippon Paint Co Ltd 表面調整用組成物及び表面調整方法
DE102008047533A1 (de) * 2008-09-16 2010-04-15 Sachtleben Chemie Gmbh Verfahren zur Herstellung von Titan-IV-phosphat
DE102011051879B4 (de) 2011-07-15 2023-11-09 Dürr Systems Ag Anlage und Verfahren zur Oberflächenbehandlung von Werkstücken sowie Verwendung einer solchen Anlage zum Lackieren von Werkstücken
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
CN103741132B (zh) * 2014-01-10 2016-08-17 湖南金裕化工有限公司 胶钛表面调整剂及其制备方法
DE102014105226A1 (de) 2014-04-11 2015-10-15 Thyssenkrupp Ag Verfahren zur Aktivierung von zu phosphatierenden Metalloberflächen, vorzugsweise verzinktem Stahlblech
CN121006536A (zh) * 2017-08-31 2025-11-25 凯密特尔有限责任公司 用于无镍磷化金属表面的改进方法
CN114990537B (zh) * 2022-08-04 2022-11-25 山东一立动力科技股份有限公司 一种铝合金表面磷化处理方法
EP4339324A1 (fr) * 2022-09-19 2024-03-20 ThyssenKrupp Steel Europe AG Produit plat en acier doté d'une couche d'activation pour le formage à chaud
EP4689227A2 (fr) * 2023-04-04 2026-02-11 Chemetall GmbH Composition de nettoyage et procédé de nettoyage de surfaces métalliques pour empêcher la corrosion d'un bain de rinçage

Family Cites Families (6)

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Publication number Priority date Publication date Assignee Title
BE410815A (fr) * 1934-08-13
US2329065A (en) * 1942-03-06 1943-09-07 Westinghouse Electric & Mfg Co Corrosion resistant coating for metal surfaces
US3166444A (en) * 1962-04-26 1965-01-19 Lubrizol Corp Method for cleaning metal articles
CA960944A (en) * 1970-11-19 1975-01-14 Dulux Australia Ltd. Grain-refining compounds
JPS5591997A (en) * 1978-12-30 1980-07-11 Nippon Parkerizing Co Ltd Surface treating method of steel plate
DE3814363A1 (de) * 1988-04-28 1989-11-09 Henkel Kgaa Titanfreie aktivierungsmittel, verfahren zu ihrer herstellung und ihre verwendung zur aktivierung von metalloberflaechen vor einer zinkphosphatierung

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008054407A1 (de) 2008-12-09 2010-06-10 Chemetall Gmbh Verfahren zur Beschichtung von metallischen Oberflächen mit einem Aktivierungsmittel vor dem Phosphatieren
WO2010066765A1 (fr) 2008-12-09 2010-06-17 Chemetall Gmbh Procédé de revêtement de surfaces métalliques au moyen d'un moyen activateur avant la phosphatation
DE102008054407B4 (de) * 2008-12-09 2018-03-29 Chemetall Gmbh Verfahren zur Beschichtung von metallischen Oberflächen mit einem Aktivierungsmittel vor dem Phosphatieren, entsprechende Aktivierungsmittel sowie Verwendung der mit dem Verfahren beschichteten Substrate
DE102018216216A1 (de) * 2018-09-24 2020-03-26 Thyssenkrupp Ag Verfahren zur Verbesserung der Phosphatierbarkeit von metallischen Oberflächen, welche mit einer temporären Vor- bzw. Nachbehandlung versehen werden
WO2021116318A1 (fr) 2019-12-13 2021-06-17 Thyssenkrupp Steel Europe Ag Procédé de production d'un produit plat en acier ayant une couche de protection métallique à base de zinc et une couche de phosphatation produite sur une surface de la couche de protection métallique, et produit plat en acier de ce type
DE102019134298A1 (de) * 2019-12-13 2021-06-17 Thyssenkrupp Steel Europe Ag Verfahren zum Herstellen eines Stahlflachprodukts mit einer metallischen Schutzschicht auf Basis von Zink und einer auf einer Oberfläche der metallischen Schutzschicht erzeugten Phosphatierschicht und derartiges Stahlflachprodukt

Also Published As

Publication number Publication date
US5160551A (en) 1992-11-03
CA2040859A1 (fr) 1991-10-22
JPH04254589A (ja) 1992-09-09
DE4012795A1 (de) 1991-10-24
EP0454211A1 (fr) 1991-10-30
ES2055518T3 (es) 1994-08-16
JP3063921B2 (ja) 2000-07-12
ZA912943B (en) 1992-12-30
ATE107711T1 (de) 1994-07-15
CA2040872A1 (fr) 1991-10-22
DE59101978D1 (de) 1994-07-28
BR9101616A (pt) 1991-12-10
CA2040859C (fr) 2000-11-21

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