EP0059994B1 - Procédé pour la fabrication de révêtements de phosphate sur des sufaces métalliques - Google Patents

Procédé pour la fabrication de révêtements de phosphate sur des sufaces métalliques Download PDF

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Publication number
EP0059994B1
EP0059994B1 EP82200190A EP82200190A EP0059994B1 EP 0059994 B1 EP0059994 B1 EP 0059994B1 EP 82200190 A EP82200190 A EP 82200190A EP 82200190 A EP82200190 A EP 82200190A EP 0059994 B1 EP0059994 B1 EP 0059994B1
Authority
EP
European Patent Office
Prior art keywords
metal surfaces
contacted
phosphating bath
phosphating
weight ratio
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
Application number
EP82200190A
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German (de)
English (en)
Other versions
EP0059994A1 (fr
Inventor
Günter Siemund
Han-Yong Dr. Dipl.-Chem. Oei
Herbert Liebl
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 Ste
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 Ste, Continentale Parker SA filed Critical Metallgesellschaft AG
Publication of EP0059994A1 publication Critical patent/EP0059994A1/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
    • C23C22/05—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
    • C23C22/14—Orthophosphates containing zinc cations containing also chlorate anions

Definitions

  • aqueous acidic zinc phosphate solutions which contain chlorate as an accelerator and additionally nitrate to apply phosphate coatings to metal surfaces by immersion or flooding.
  • chlorate-containing zinc phosphate solutions a weight ratio of P 2 O 5 : Zn in the range of approximately 1: (0.2 to 0.7) is usually maintained (cf., for example, DE-OS 21 06 626).
  • calcium ions in such solutions in order to refine the phosphate layer (cf. for example DE-PS 10 96 152).
  • the treatment time until the formation of a closed phosphate layer on the metal surfaces is extended.
  • the object of the invention is to further improve the known method, in particular the aforementioned method, so that its use leads to phosphate layers which, in particular with regard to their thickness and intergrowth, meet the highest requirements.
  • Phosphating baths which only contain chlorate as accelerators can be used in the process according to the invention. In this case, its content must be at least 1.0 g / I (calculated as CI0 3 ). If the phosphating bath also contains nitrate ions, the total of chlorate and nitrate ions must be at least 1.0 g / l. The nitrate content is determined as the oxidation equivalent based on chlorate.
  • a phosphating bath is preferably used which contains up to 5 g / l of chlorate, in particular 0.2 to 2 g / l of chlorate.
  • Another preferred embodiment of the invention consists in bringing the metal surfaces into contact with a phosphating bath which contains 5 to 20 g / 1 sulfate ions.
  • a phosphating bath which contains 5 to 20 g / 1 sulfate ions.
  • Concentrates are expediently used to prepare and supplement the phosphating bath used in the procedure according to the invention. It is advantageous to design them in such a way that - apart from the sulfate content - they contain as many components as possible. It is advisable to add the sulfate separately.
  • the phosphating bath 5 contain up to 1000 mg / l Ni and / or 1 to 50 mg / 1 Cu ions.
  • the workpieces to be treated must be free of rust and scale.
  • a possible course of treatment is, for example: degreasing with organic solvents or alkaline cleaners (the latter is then rinsed with water), pickling in mineral acids, such as HCI or H 2 S0 4 , to remove scale and rust, rinsing with cold water.
  • the workpieces can then according to the inventive method at temperatures between 35 and 98 ° C and. a bath number of at least 20 5 to 15 minutes in diving or flooding.
  • the phosphating bath is supplemented with the supplementary concentrate mentioned.
  • the surface of the workpieces can be activated by pre-rinsing with hot water or with activating titanium orthophosphate dispersions. After phosphating, the workpieces are rinsed with cold water and can then be treated with passivating rinse solutions or, in the case of cold-formed parts, with lubricants and, if necessary, lubricant carrier salts such as borax or lime.
  • the method according to the invention has proven particularly useful as a preparation for non-cutting cold forming. However, it is also advantageous in the other fields of application of phosphating, e.g. Use corrosion protection, to facilitate sliding friction.
  • the phosphating baths had the following composition:
  • the phosphate layers produced using baths containing sulfate ions are of considerably greater thickness.

Landscapes

  • 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)

Claims (6)

1. Procédé de fabrication de revêtements de phosphate sur des surfaces métalliques, en particulier de fer et d'acier, à 35 à 98°C par le procédé d'immersion ou d'arrosage, avec une solution aqueuse, acide, de phosphate de zinc contenant comme accélérateur du chlorate, et les cas échéant du nitrate, qui contient au moins 6 g/l de zinc, au moins 5 g/l de P2O5, au moins 1,0 g/I d'accélérateur (calculé en CI03), qui présente un nombre de points d'acidité totale d'au moins 20 et dans laquelle le rapport pondéral P205 libre : P205 total = (0,2 à 0,6) : 1, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation dans lequel le rapport pondéral P205 : Zn : ClO3 = 1 : (0,5 à 4,0) : (0,01 à 1,0) et qui contient en outre de 1 à 50 g/I d'ions sulfate.
2. Procédé suivant la revendication 1, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation dans lequel la teneur en chlorate est jusqu'à 5 g/l, de préférence de 0,2 à 2 g/1 (calculée en CI03). '
3. Procédé suivant la revendication 1 ou 2, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation qui contient de 5 à 20 g/I d'ions sulfate.
4. Procédé suivant la revendication 1, 2 ou 3, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation dans lequel le rapport pondéral P205 : No3 = 1 : (0,2 à 6).
5. Procédé suivant la revendication 1, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation qui est enrichi conformément à un rapport pondéral P205 : Zn : N03 : ClO3 = 1 : (0,36 à 0,80) : (0,10 à 0,60) : (0,15 à 0,60) ainsi que P205 libre : P205 total = (0,20 à 0,70): 1.
6. Procédé suivant une ou plusieurs des revendications 1 à 4, caractérisé en ce qu'on met en contact les surfaces métalliques avec un bain de phosphatation qui contient de 5 à 1.000 mg/I d'ions Ni et/ou de 1 à 50 mg/l d'ions Cu.
EP82200190A 1981-03-06 1982-02-18 Procédé pour la fabrication de révêtements de phosphate sur des sufaces métalliques Expired EP0059994B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3108484 1981-03-06
DE19813108484 DE3108484A1 (de) 1981-03-06 1981-03-06 Verfahren zur herstellung von phosphatueberzuegen auf metalloberflaechen

Publications (2)

Publication Number Publication Date
EP0059994A1 EP0059994A1 (fr) 1982-09-15
EP0059994B1 true EP0059994B1 (fr) 1984-12-27

Family

ID=6126487

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82200190A Expired EP0059994B1 (fr) 1981-03-06 1982-02-18 Procédé pour la fabrication de révêtements de phosphate sur des sufaces métalliques

Country Status (7)

Country Link
US (1) US4416705A (fr)
EP (1) EP0059994B1 (fr)
JP (1) JPS6045705B2 (fr)
CA (1) CA1175606A (fr)
DE (2) DE3108484A1 (fr)
GB (1) GB2094356B (fr)
IT (1) IT1150234B (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3245411A1 (de) * 1982-12-08 1984-07-05 Gerhard Collardin GmbH, 5000 Köln Verfahren zur phosphatierung elektrolytisch verzinkter metallwaren
JPS619580A (ja) * 1984-06-25 1986-01-17 Nippon Parkerizing Co Ltd 黒色化リン酸塩処理方法
CA1257527A (fr) * 1984-12-20 1989-07-18 Thomas W. Tull Procede de deformation a froid avec enduction lubrifiante amelioree
JPS63270478A (ja) * 1986-12-09 1988-11-08 Nippon Denso Co Ltd リン酸塩化成処理方法
EP0327153B1 (fr) * 1988-02-03 1993-08-04 Metallgesellschaft Ag Procédé pour former des couches de phosphates sur des métaux
IT1295500B1 (it) * 1997-10-21 1999-05-12 Pierangelo Girardello Procedimento per la lavorazione dei metalli e prodotto ottenuto con detto procedimento.
WO2018039462A1 (fr) 2016-08-24 2018-03-01 Ppg Industries Ohio, Inc. Composition alcaline destiné au traitement de substrats métalliques

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1159728B (de) * 1954-04-24 1963-12-19 Metallgesellschaft Ag Verfahren zum Aufbringen von Phosphatueberzuegen
DE1231523B (de) * 1962-03-20 1966-12-29 Metallgesellschaft Ag Verfahren zur Verbesserung eines zur elektrischen Isolierung auf Blechen und Baendern aus Eisen und Stahl aufgebrachten Phosphatueberzugs
DE1521879B2 (de) * 1966-07-12 1975-08-28 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zum Aufbringen von Phosphatüberzügen auf Eisen und Stahl
DE1796102A1 (de) * 1968-08-31 1972-02-17 Metallgesellschaft Ag Verfahren zum Aufbringen eines Phosphatueberzuges auf Oberflaechen von Eisen und Stahl
DE2106626A1 (de) * 1970-03-04 1971-09-23 Metallgesellschaft Ag Verfahren zur Herstellung eines Phosphatüberzuges auf Metalloberflächen
GB1296883A (fr) * 1970-03-04 1972-11-22
BE788795A (fr) * 1971-09-20 1973-01-02 Parker Ste Continentale Procede de formation d'un revetement de phosphate sur une surface metallique
US4071379A (en) * 1976-01-28 1978-01-31 Imperial Chemical Industries Limited Phosphating method
JPS5811515B2 (ja) * 1979-05-11 1983-03-03 日本ペイント株式会社 金属表面にリン酸亜鉛皮膜を形成するための組成物

Also Published As

Publication number Publication date
DE3108484A1 (de) 1982-09-23
IT1150234B (it) 1986-12-10
JPS57152473A (en) 1982-09-20
EP0059994A1 (fr) 1982-09-15
IT8219938A0 (it) 1982-03-03
CA1175606A (fr) 1984-10-09
US4416705A (en) 1983-11-22
DE3261654D1 (en) 1985-02-07
GB2094356A (en) 1982-09-15
GB2094356B (en) 1984-08-08
JPS6045705B2 (ja) 1985-10-11

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