EP0717787B1 - Procede de phosphatage sans nickel - Google Patents

Procede de phosphatage sans nickel Download PDF

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Publication number
EP0717787B1
EP0717787B1 EP94925483A EP94925483A EP0717787B1 EP 0717787 B1 EP0717787 B1 EP 0717787B1 EP 94925483 A EP94925483 A EP 94925483A EP 94925483 A EP94925483 A EP 94925483A EP 0717787 B1 EP0717787 B1 EP 0717787B1
Authority
EP
European Patent Office
Prior art keywords
phosphating
hydroxylamine
free
phosphating solution
ions
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
EP94925483A
Other languages
German (de)
English (en)
Other versions
EP0717787A1 (fr
Inventor
Wolf-Achim Roland
Karl-Heinz Gottwald
Karl Dieter Brands
Jan-Willem Brouwer
Bernd Mayer
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
Priority claimed from DE4330104A external-priority patent/DE4330104A1/de
Priority claimed from DE19934341041 external-priority patent/DE4341041A1/de
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0717787A1 publication Critical patent/EP0717787A1/fr
Application granted granted Critical
Publication of EP0717787B1 publication Critical patent/EP0717787B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
    • C23C22/44—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—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
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/13—Orthophosphates containing zinc cations containing also nitrate or nitrite anions
    • 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
    • C23C22/34—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
    • C23C22/364—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 also manganese 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
    • C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
    • C23C22/42—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also phosphates

Claims (16)

  1. Procédé pour le phosphatage de surfaces métalliques à l'aide de solutions de phosphatage acides aqueuses qui contiennent des ions zinc, manganèse et phosphate et, à titre d'accélérateurs, de l'hydroxylamine ou un composé d'hydroxylamine et/ou de l'acide m-nitrobenzosulfonique ou encore ses sels hydrosolubles, caractérisé en ce qu'on amène les surfaces métalliques en contact avec une solution de phosphatage qui est exempte de nickel, de cobalt, de cuivre, de nitrite et d'oxo-anions d'halogènes dans le sens où ces éléments, respectivement ces ions ne sont pas ajoutés au bain de manière délibérée, la concentration en nickel étant inférieure à 0,01 g/l, et qui contient
    de 0,3 à 2 g/l de Zn(II),
    de 0,3 à 4 g/l de Mn(II),
    de 5 à 40 g/l d'ions phosphate,
    de 0,1 à 5 g/l d'hydroxylamine sous forme libre ou sous forme liée et/ou
    de 0,2 à 2 g/l de m-nitrobenzènesulfonate
    et au maximum 0,5 g/l d'ions nitrate,
    la teneur en Mn représentant au moins 50% de la teneur en Zn.
  2. Procédé selon la revendication 1, caractérisé en ce que la solution de phosphatage contient moins de 0,1 g/l de nitrate.
  3. Procédé selon une des revendications 1 et 2 ou selon les deux, caractérisé en ce que la solution de phosphatage contient en outre du fluorure sous forme libre et/ou sous forme liée pour obtenir un complexe dans des quantités allant jusqu'à 2,5 g/l de fluorure total, dont le fluorure libre représente une quantité allant jusqu'à 800 g/l.
  4. Procédé selon une ou plusieurs des revendications 1 à 3, caractérisé en ce que la solution de phosphatage présente un rapport pondéral des ions phosphate aux ions zinc entre 3,7 et 30, de préférence entre 10 et 20.
  5. Procédé selon une ou plusieurs des revendications 1 à 4, caractérisé en ce que la solution de phosphatage présente une teneur en Mn(II) entre 0,3 et 2 g/l, de préférence entre 0,5 et 1,5 g/l.
  6. Procédé selon une ou plusieurs des revendications 1 à 5, caractérisé en ce que la solution de phosphatage contient du m-nitrobenzènesulfonate comme acide libre ou comme sel hydrosoluble, en particulier comme sel de sodium, et la concentration en m-nitrobenzènesulfonate s'élève de préférence de 0,4 à 1 g/l.
  7. Procédé selon une ou plusieurs des revendications 1 à 6, caractérisé en ce que la valeur de l'acide total se situe entre 15 et 25 points et la valeur de l'acide libre lors d'un phosphatage partiel s'élève entre 0,3 et 1,5 point; dans le cas d'un phosphatage de rubans, entre 0,3 et 2,5 points.
  8. Procédé selon une ou plusieurs des revendications 1 à 7, caractérisé en ce que la solution de phosphatage contient de l'hydroxylamine sous forme libre ou sous forme liée pour obtenir un complexe ou encore sous forme de ses sels, en particulier sous forme des sulfates ou des phosphates.
  9. Procédé selon la revendication 8, caractérisé en ce que la solution de phosphatage présente une teneur en hydroxylamine sous forme libre, sous forme de sels ou sous forme liée pour obtenir un complexe entre 0,4 et 2 g/l calculés comme hydroxylamine.
  10. Procédé selon une des revendications 8 et 9 ou selon les deux, caractérisé en ce que le rapport de la somme des concentrations du zinc et du manganèse à la concentration de l'hydroxylamine s'élève, respectivement en g/l, de 1,0 à 6,0, de préférence de 2,0 à 4,0.
  11. Procédé selon une ou plusieurs des revendications 8 à 10, caractérisé en ce que la solution de phosphatage contient en outre de 20 à 800 mg/l, de préférence de 50 à 600 mg/l de tungstène sous forme de tungstates, de silicotungstates et/ou de borotungstates hydrosolubles, sous forme de leurs acides et/ou sous forme de leurs sels d'ammonium, de métaux alcalins et/ou de métaux alcalino-terreux.
  12. Procédé selon une ou plusieurs des revendications 1 à 11, caractérisé en ce que la solution de phosphatage contient, soit de l'hydroxylamine, soit de l'acide m-nitrobenzènesulfonique.
  13. Procédé selon une ou plusieurs des revendications 1 à 12, pour le traitement de surfaces en acier, en acier galvanisé ou en acier allié galvanisé, en aluminium, en acier aluminé ou en acier allié aluminé.
  14. Procédé selon la revendication 13, caractérisé en ce qu'on amène la surface métallique en contact avec la solution de phosphatage par pulvérisation, par trempage ou encore par pulvérisation-trempage pendant des temps de traitement entre 5 secondes et 8 minutes.
  15. Procédé selon la revendication 14, caractérisé en ce que la température de la solution de phosphatage se situe entre 30 et 70°C.
  16. Procédé selon la revendication 15, pour le traitement de surfaces métalliques avant une mise en peinture, en particulier avant un trempage électrophorétique de type cathodique.
EP94925483A 1993-09-06 1994-08-29 Procede de phosphatage sans nickel Expired - Lifetime EP0717787B1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE4330104 1993-09-06
DE4330104A DE4330104A1 (de) 1993-09-06 1993-09-06 Nickel- und Kupfer-freies Phosphatierverfahren
DE4341041 1993-12-02
DE19934341041 DE4341041A1 (de) 1993-12-02 1993-12-02 Nickelfreies Phosphatierverfahren mit m-Nitrobenzolsulfonat
PCT/EP1994/002848 WO1995007370A1 (fr) 1993-09-06 1994-08-29 Procedes de phosphatage sans nickel

Publications (2)

Publication Number Publication Date
EP0717787A1 EP0717787A1 (fr) 1996-06-26
EP0717787B1 true EP0717787B1 (fr) 1998-01-14

Family

ID=25929280

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94925483A Expired - Lifetime EP0717787B1 (fr) 1993-09-06 1994-08-29 Procede de phosphatage sans nickel

Country Status (13)

Country Link
US (1) US5792283A (fr)
EP (1) EP0717787B1 (fr)
JP (1) JP3348856B2 (fr)
KR (1) KR100327287B1 (fr)
CN (1) CN1041001C (fr)
AT (1) ATE162233T1 (fr)
AU (1) AU678284B2 (fr)
BR (1) BR9407485A (fr)
CA (1) CA2171180A1 (fr)
CZ (1) CZ286514B6 (fr)
DE (1) DE59405046D1 (fr)
ES (1) ES2111949T3 (fr)
WO (1) WO1995007370A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103184444A (zh) * 2013-03-29 2013-07-03 柳州煜华科技有限公司 一种适用于金属紧固件的磷化液

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US5653790A (en) * 1994-11-23 1997-08-05 Ppg Industries, Inc. Zinc phosphate tungsten-containing coating compositions using accelerators
DE19511573A1 (de) * 1995-03-29 1996-10-02 Henkel Kgaa Verfahren zur Phosphatierung mit metallhaltiger Nachspülung
DE19639596A1 (de) * 1996-09-26 1998-04-02 Henkel Kgaa Verfahren zur Phosphatierung von Stahlband
DE19756735A1 (de) * 1997-12-19 1999-06-24 Henkel Kgaa Phosphatierung von einseitig verzinktem Stahlband
DE19808440C2 (de) 1998-02-27 2000-08-24 Metallgesellschaft Ag Wässrige Lösung und Verfahren zur Phosphatierung metallischer Oberflächen sowie eine Verwendung der Lösung und des Verfahrens
DE19808755A1 (de) 1998-03-02 1999-09-09 Henkel Kgaa Schichtgewichtsteuerung bei Bandphosphatierung
DE19834796A1 (de) 1998-08-01 2000-02-03 Henkel Kgaa Verfahren zur Phosphatierung, Nachspülung und kathodischer Elektrotauchlackierung
AU2348500A (en) * 1998-12-23 2000-07-31 Henkel Corporation Composition and process for heavy zinc phosphating
JP2001342575A (ja) * 2000-05-31 2001-12-14 Nippon Dacro Shamrock Co Ltd 水性金属表面処理剤
DE10110833B4 (de) * 2001-03-06 2005-03-24 Chemetall Gmbh Verfahren zum Aufbringen eines Phosphatüberzuges und Verwendung der derart phosphatierten Metallteile
DE10155666A1 (de) * 2001-11-13 2003-05-22 Henkel Kgaa Mit Hydroxylamin und organischen Stickstoffverbindungen beschleunigtes Phosphatierverfahren
KR100554740B1 (ko) * 2001-12-17 2006-02-24 주식회사 포스코 인산피막이 형성된 전기아연 도금강판 제조방법
CA2686179A1 (fr) * 2007-06-07 2009-02-05 Henkel Ag & Co. Kgaa Phosphatation au manganese, zinc et modifiee au cobalt
DE102010001686A1 (de) 2010-02-09 2011-08-11 Henkel AG & Co. KGaA, 40589 Zusammensetzung für die alkalische Passivierung von Zinkoberflächen
EP2503025B1 (fr) 2011-03-22 2013-07-03 Henkel AG & Co. KGaA Traitement en plusieurs étapes de protection contre la corrosion des pièces métalliques ayant au moins partiellement une surface en zinc ou en alliages de zinc
CN102703889B (zh) * 2012-05-28 2014-06-04 武汉永正科技发展有限公司 低温单组份锌系磷化液及其制备方法
CN104651820A (zh) * 2015-02-16 2015-05-27 天津大学 一种碳钢超声磷化液及制备方法以及采用磷化液对碳钢磷化的方法
ES2873381T3 (es) * 2015-04-07 2021-11-03 Chemetall Gmbh Procedimiento para el ajuste específico de la conductividad eléctrica de revestimientos de conversión

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ATE160592T1 (de) * 1985-08-27 1997-12-15 Henkel Corp Verfahren zur phosphatierung von metalloberflächen
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103184444A (zh) * 2013-03-29 2013-07-03 柳州煜华科技有限公司 一种适用于金属紧固件的磷化液
CN103184444B (zh) * 2013-03-29 2016-08-03 柳州煜华科技有限公司 一种适用于金属紧固件的磷化液

Also Published As

Publication number Publication date
CZ67396A3 (en) 1996-12-11
JP3348856B2 (ja) 2002-11-20
KR960705076A (ko) 1996-10-09
CA2171180A1 (fr) 1995-03-16
WO1995007370A1 (fr) 1995-03-16
CN1041001C (zh) 1998-12-02
KR100327287B1 (ko) 2002-11-22
CN1129961A (zh) 1996-08-28
AU678284B2 (en) 1997-05-22
BR9407485A (pt) 1996-06-25
CZ286514B6 (cs) 2000-05-17
US5792283A (en) 1998-08-11
JPH09502224A (ja) 1997-03-04
ES2111949T3 (es) 1998-03-16
EP0717787A1 (fr) 1996-06-26
ATE162233T1 (de) 1998-01-15
DE59405046D1 (de) 1998-02-19
AU7537394A (en) 1995-03-27

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