EP1019564A1 - Procede de phosphatation d'un feuillard d'acier - Google Patents

Procede de phosphatation d'un feuillard d'acier

Info

Publication number
EP1019564A1
EP1019564A1 EP98949988A EP98949988A EP1019564A1 EP 1019564 A1 EP1019564 A1 EP 1019564A1 EP 98949988 A EP98949988 A EP 98949988A EP 98949988 A EP98949988 A EP 98949988A EP 1019564 A1 EP1019564 A1 EP 1019564A1
Authority
EP
European Patent Office
Prior art keywords
phosphating
ions
range
free
steel strip
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.)
Ceased
Application number
EP98949988A
Other languages
German (de)
English (en)
Inventor
Jörg Riesop
Reinhard Seidel
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP1019564A1 publication Critical patent/EP1019564A1/fr
Ceased legal-status Critical Current

Links

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
    • C23C22/07—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
    • C23C22/18—Orthophosphates containing manganese cations
    • C23C22/182—Orthophosphates containing manganese cations containing also zinc cations
    • 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
    • C23C22/18—Orthophosphates containing manganese cations
    • C23C22/188—Orthophosphates containing manganese cations containing also magnesium cations
    • 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
    • C23C22/36—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 phosphates
    • C23C22/368—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 phosphates containing magnesium cations

Definitions

  • the invention relates to a method for phosphating steel strip or steel strip galvanized on one or both sides or alloy galvanized by spraying or immersion treatment, which takes place for a period of time in the range of approximately 2 to approximately 20 seconds, depending on the strip speed.
  • phosphating surfaces made of iron, steel, zinc and their alloys as well as aluminum and its alloys have long been state of the art.
  • the phosphating of the surfaces mentioned serves to increase the adhesive strength of paint layers and to improve corrosion protection.
  • the phosphating is carried out by immersing the metal surfaces in the phosphating solutions or by spraying the metal surfaces with the phosphating solutions. Combined methods are also known.
  • Shaped metal parts such as automobile bodies can be phosphated, but also metal strips in high-speed conveyor systems.
  • the present invention is concerned with such a band phosphating.
  • Belt phosphating differs from partial phosphating in that, because of the high belt speeds, the phosphating, i.e. H. the growth of a closed metal phosphate layer must take place within a short period of time, for example about 2 to about 20 seconds.
  • WO 91/02829 describes a method for Phosphating of electrolytically and / or hot-dip galvanized steel strip through short-term treatment with acid phosphating solutions, which, in addition to zinc and phosphate ions, contain manganese and nickel cations as well as anions containing oxygen
  • DE-A-35 37 108 also describes a process for the phosphating of electrolytically galvanized steel strips
  • Phosphate ions other metal cations such as nickel ions and / or
  • Nitrate ions included.
  • the contents of zinc cations are in the relatively low range of 0.1 to 0.8 g / 1.
  • DE-A-39 20 296 describes a process for the production of zinc phosphate coatings containing manganese and magnesium on steel, zinc, aluminum and / or their alloys by spraying, spray-immersion and / or immersion with an aqueous solution which is 0.2 to 1.0 g / 1 zinc ions, 0.2 to 2.0 g / 1 manganese ions, 0.5 to 2 g / 1 magnesium ions, 10 to 20 g / 1 phosphate ions, 0.2 to 10 g / 1 nitrate ions and up to Contains 1.0 g / 1 fluoride ions.
  • This phosphating solution also necessarily contains as accelerator: 0.02 to 0.2 g / 1 nitrite ion and / or 0.4 to 1 g / 1 chlorate ion and / or 0.2 to 1 g / 1 of an organic oxidizing agent.
  • the nitrate ions necessary in this process can lead to a loss of quality of the phosphate layer on galvanized steel surfaces due to speck formation.
  • "specks" are understood to be whitish corrosion points on the metal surface which show a crater-like appearance in microscopic images. From the phosphating times of more than 2 minutes mentioned in the exemplary embodiments, it can be seen that this is not a process for band phosphating.
  • German patent application 196 39 596 attempts to provide a phosphating process which, on the one hand, solves the problem of speck formation and, on the other hand, enables even galvanized steel strips or the non-galvanized side of steel strips galvanized on one side in the short phosphating times customary in strip systems with a closed crystalline phosphate layer Mistake.
  • this object is achieved by a method for phosphating steel strip or steel strip galvanized on one or both sides or alloy galvanized by spraying or dipping treatment for a period of time in the range from 2 to 15 seconds with an acidic, zinc and manganese-containing phosphating solution with a Temperature in the range from 40 to 70 ° C, characterized in that the phosphating solution contains 1 to 4 g / 1 zinc ions,
  • the object of the invention is therefore to provide a phosphating process for high-speed conveyor systems with phosphating times in the range from about 2 to about 20 seconds, which on the one hand works nickel-free and on the other hand leads to phosphate layers, the quality of which does not protect those of nickel-containing phosphate layers in terms of corrosion protection and paint adhesion is inferior.
  • This object is achieved by a method for phosphating steel strip or steel strip galvanized on one or both sides or galvanized with alloys by spraying or dipping treatment for a period of time in the range from 2 to 20 seconds with an acidic, zinc, magnesium and manganese-containing phosphating solution with a temperature in the range of 50 to 70 ° C, thereby characterized in that the phosphating solution is free of nitrate ions and that it
  • the steel strips can be galvanized or hot-dip galvanized or alloy-galvanized.
  • “Galvanized alloy” is understood to mean that the steel surface has been coated with an alloy which, in addition to zinc, contains other metals such as iron, nickel or aluminum.
  • An alloy galvanizing with a zinc-iron alloy can take place, for example, by tempering a galvanized steel strip , which causes a diffusion of iron atoms into the zinc layer and vice versa.
  • the layer thicknesses of the galvanizing layers are usually in the range from about 5 to about 20 ⁇ m.
  • free acid and total acid are generally known in the field of phosphating. They are determined by titrating the acid bath sample with 0.1 normal sodium hydroxide solution and measuring its consumption. The consumption in ml is given as a score.
  • the number of free acids means the consumption in ml of 0.1 normal sodium hydroxide solution in order to titrate 10 ml of bath solution, which has been diluted to 50 ml with deionized water, up to a pH of 4.0 .
  • the total acid score indicates consumption in ml up to a pH of 8.2.
  • the free acid is set to the range 1.5 to 2.8 points, the total acid to the range 25 to 35 points.
  • Hydroxylamine can be used as a free base, as a hydroxylamine-releasing compound such as hydroxylamine complexes and ketoximes or aldoximes or in the form of hydroxylammonium salts. If free hydroxylamine is added to the phosphating bath or a phosphating bath concentrate, it will largely exist as a hydroxylammonium cation due to the acidic nature of these solutions. When used as a hydroxylammonium salt, the sulfates and the phosphates are particularly suitable. In the case of the phosphates, the acid salts are preferred due to the better solubility.
  • a combination of free hydroxyamine and hydroxylammonium sulfate can advantageously be used to take into account economic aspects on the one hand and on the other hand to not burden the phosphating baths with too much sulfate ions.
  • Hydroxylamine or its compounds are added to the phosphating solution in amounts such that the calculated concentration of the free hydroxylamine is between about 0.1 to about 3 g / 1, preferably between about 0.15 and about 1 g / 1.
  • the total phosphorus content of the phosphating bath is considered to be present in the form of phosphate ions POz ⁇ -. Accordingly, the known fact that the pH values of the phosphating baths in the range from about 2.0 to about 3.6, which are in the acidic region, only a very small part of the phosphate is actually in the form is ignored when calculating or determining the concentration the triple negatively charged anions are present. At these pH values it is rather to be expected that the phosphate is present primarily as a simply negatively charged dihydrogenphosphate anion, together with undisociated phosphoric acid and with smaller amounts of double negatively charged hydrogen phosphate anions.
  • the phosphating solution should not contain more than about 0.05 g / 1 nickel ion and in particular not more than about 0.015 g / 1 nickel ion.
  • the phosphating solutions contain alkali metal and / or ammonium cations in order to adjust the value of the free acid to the desired range.
  • a further preferred embodiment of the invention consists in using phosphating solutions which contain up to about 0.8 g / 1 fluoride in free or complex-bound form.
  • the preferred fluoride contents are in the range from 0.0 to about 0.5 g / 1, in particular in the range from about 0.1 to about 0.2 g / 1.
  • the phosphating solutions are generally prepared in the manner known to the person skilled in the art.
  • phosphate is introduced into the phosphating solutions in the form of phosphoric acid.
  • the cations are added in the form of acid-soluble compounds such as, for example, the carbonates, the oxides or the hydroxides of phosphoric acid, so that this is partially neutralized.
  • the further neutralization to the desired pH range is preferably carried out by adding sodium hydroxide or sodium carbonate.
  • Suitable sources of free fluoride anions are, for example, sodium or potassium fluoride.
  • tetrafluoroborate or hexafluorosilicate can be used as complex fluorides.
  • the invention relates to the use of the phosphating method described above for the production of phosphate layers on both sides with a mass per unit area in the range from approximately 0.4 to approximately 2.0 g / m 2 on steel strip or on steel strip galvanized or alloy-galvanized on one or both sides .
  • Phosphate layers with a mass per unit area in the range from approximately 0.9 to approximately 1.8 g / m 2 are preferably produced.
  • the mass per unit area (“layer weight”) can, as is known to the person skilled in the art, be determined by weighing a phosphated sample sheet, detaching the phosphate layer in 5% chromic acid solution and weighing the sample sheet back. This method is described, for example, in DIN 50942.
  • phosphating solutions are preferably used, the free acid content of which is in the range from approximately 1.5 to approximately 2.8 points and the total acid content is in the range of approximately 25 to approximately 35 points Range from about 50 to about 70 ° C. and in particular in the range from about 55 to about 65 ° C. Preferred treatment times are in the range from about 5 to about 10 seconds.
  • the phosphating solution is preferably sprayed onto the metal surface and rinsed off with water after the desired treatment time.
  • the metal surface must be completely water wettable before applying the phosphating solution. This is usually the case in continuously operating conveyor systems. However, if the belt surface is oiled, this oil must be removed by a suitable cleaner before phosphating. The procedures for this are common in the art.
  • activation is usually carried out using activation agents known in the art. Solutions or suspensions are usually used which contain titanium phosphates and sodium phosphates. The activation is followed by the use of the phosphating process according to the invention, which is advantageously followed by a passivating rinse. An intermediate rinse with water usually takes place between phosphating and passivating rinsing. Treatment baths containing chromic acid are widely used for passivating rinsing.
  • the metal tapes according to the invention can be phosphated directly with an organic coating. However, you can also in the initially unpainted state after cutting, shaping and joining to components such as Automobile bodies or household appliances are put together. The associated forming processes are facilitated by the phosphate layer. If the finished components have a low corrosive stress, such as in household appliances, the devices assembled from the pre-phosphated metal can be painted directly. For higher corrosion protection requirements, such as those made in automobile construction, it is advantageous to have a phosphating treatment again after assembling the bodies.

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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 procédé de phosphatation d'un feuillard d'acier ou d'un feuillard d'acier zingué ou galvanisé par dépôt d'alliage sur une ou deux faces, par pulvérisation ou par immersion, pendant 2 à 20 secondes, avec une solution de phosphatation acide, contenant du zinc, du magnésium et du manganèse, à une température de l'ordre de 50 à 70 DEG C. Ce procédé se caractérise en ce que la solution de phosphatation ne comprend pas d'ions de nitrate et qu'elle contient: entre 1 et 4 g/l d'ions de zinc, entre 1,2 et 4 g/l d'ions de manganèse, entre 1 et 4 g/l d'ions de magnésium, entre 10 et 30 g/l d'ions de phosphate, entre 0,1 et 3 g/l d'hydroxylamine sous forme libre, ionique ou liée. La teneur en acide de cette solution de phosphatation se situe entre 0,4 et 4 points et sa teneur en acide total est de l'ordre de 15 à 45 points.
EP98949988A 1997-09-17 1998-09-05 Procede de phosphatation d'un feuillard d'acier Ceased EP1019564A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE1997140953 DE19740953A1 (de) 1997-09-17 1997-09-17 Verfahren zur Phosphatierung von Stahlband
DE19740953 1997-09-17
PCT/EP1998/005634 WO1999014397A1 (fr) 1997-09-17 1998-09-05 Procede de phosphatation d'un feuillard d'acier

Publications (1)

Publication Number Publication Date
EP1019564A1 true EP1019564A1 (fr) 2000-07-19

Family

ID=7842689

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98949988A Ceased EP1019564A1 (fr) 1997-09-17 1998-09-05 Procede de phosphatation d'un feuillard d'acier

Country Status (4)

Country Link
EP (1) EP1019564A1 (fr)
CA (1) CA2303877A1 (fr)
DE (1) DE19740953A1 (fr)
WO (1) WO1999014397A1 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19808755A1 (de) 1998-03-02 1999-09-09 Henkel Kgaa Schichtgewichtsteuerung bei Bandphosphatierung
US6596414B1 (en) * 1999-05-27 2003-07-22 Nippon Steel Corporation Phosphate-treated galvanized steel sheet excellent in corrosion resistance and paintability
TW475002B (en) 1999-07-08 2002-02-01 Kawasaki Steel Co Perforative corrosion resistant galvanized steel sheet
CA2381561C (fr) * 1999-08-09 2007-02-20 Nippon Steel Corporation Plaque d'acier en metal a base de zinc traitee avec un phosphate a formabilite excellente et son procede d'obtention
DE10110833B4 (de) * 2001-03-06 2005-03-24 Chemetall Gmbh Verfahren zum Aufbringen eines Phosphatüberzuges und Verwendung der derart phosphatierten Metallteile
DE102006035779B4 (de) * 2006-08-01 2017-01-12 Schaeffler Technologies AG & Co. KG Verfahrung zur Herstellung einer Laufscheibe eines Riementriebes
WO2013160566A1 (fr) 2012-04-25 2013-10-31 Arcelormittal Investigacion Y Desarrollo, S.L. Procédé de réalisation d'une tôle à revêtements znalmg huilés et tôle correspondante.
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

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3920296A1 (de) * 1989-06-21 1991-01-10 Henkel Kgaa Verfahren zur herstellung von mangan- und magnesiumhaltigen zinkphosphatueberzuegen
DE4013483A1 (de) * 1990-04-27 1991-10-31 Metallgesellschaft Ag Verfahren zur phosphatierung von metalloberflaechen
US5328526A (en) * 1992-04-03 1994-07-12 Nippon Paint Co., Ltd. Method for zinc-phosphating metal surface
JPH05287549A (ja) * 1992-04-03 1993-11-02 Nippon Paint Co Ltd カチオン型電着塗装のための金属表面のリン酸亜鉛処理方法
BR9307702A (pt) * 1992-12-22 1999-08-31 Henkel Corp Composição lìquida aquosa, e, processo para a produção de um revestimento de fosfato e um revestimento protetor sobre a superfìcie de um substrato metálico
DE4341041A1 (de) * 1993-12-02 1995-06-08 Henkel Kgaa Nickelfreies Phosphatierverfahren mit m-Nitrobenzolsulfonat
DE19538778A1 (de) * 1995-10-18 1997-04-24 Henkel Kgaa Schichtgewichtssteuerung bei Hydroxylamin-beschleunigten Phosphatiersystemen
DE19621184A1 (de) * 1996-05-28 1997-12-04 Henkel Kgaa Zinkphosphatierung mit integrierter Nachpassivierung
DE19639596A1 (de) * 1996-09-26 1998-04-02 Henkel Kgaa Verfahren zur Phosphatierung von Stahlband

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9914397A1 *

Also Published As

Publication number Publication date
DE19740953A1 (de) 1999-03-18
WO1999014397A1 (fr) 1999-03-25
CA2303877A1 (fr) 1999-03-25

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