EP0312176B1 - Procédé pour produire des couches de conversion - Google Patents

Procédé pour produire des couches de conversion Download PDF

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Publication number
EP0312176B1
EP0312176B1 EP88202291A EP88202291A EP0312176B1 EP 0312176 B1 EP0312176 B1 EP 0312176B1 EP 88202291 A EP88202291 A EP 88202291A EP 88202291 A EP88202291 A EP 88202291A EP 0312176 B1 EP0312176 B1 EP 0312176B1
Authority
EP
European Patent Office
Prior art keywords
tin
solution
coating
treatment
conversion
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
EP88202291A
Other languages
German (de)
English (en)
Other versions
EP0312176A1 (fr
Inventor
Yasunobu Matsushima
Shigeo Tanaka
Tomoyuki Aoki
Yohiji Ono
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.)
Nihon Parkerizing Co Ltd
Original Assignee
Nihon Parkerizing Co Ltd
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 Nihon Parkerizing Co Ltd filed Critical Nihon Parkerizing Co Ltd
Publication of EP0312176A1 publication Critical patent/EP0312176A1/fr
Application granted granted Critical
Publication of EP0312176B1 publication Critical patent/EP0312176B1/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
    • C23C22/07—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
    • C23C22/10—Orthophosphates containing oxidants
    • 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
    • C23C22/23—Condensed phosphates
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/36—Phosphatising

Definitions

  • a disadvantage of using these known solutions is that when the treatment systems are at a standstill, the tin content in the solution drops, so that conversion coatings of inferior quality are produced when the system is restarted, unless an additional addition of tin to the treatment solution is carried out beforehand.
  • a method for cathodic deposition of a phosphate coating on stainless steels in which a phosphating solution is used which contains a chelating agent, such as condensed phosphates.
  • the object of the invention is to provide a process for applying conversion coatings on tinplate which does not have the disadvantages of the known processes and which, with small tin deposits, leads to conversion coatings with excellent corrosion resistance and precludes a decrease in the tin concentration in the treatment solution when the treatment systems are at a standstill.
  • the complexing agent content suppressed the tin precipitation from the treatment solution, but at the same time its deposition on the workpiece surface when the Conversion overlay is not prevented.
  • the complexing agent also accelerates the pickling attack on the metal surface and is responsible for a balance between the tin which dissolves (as a result of the pickling attack) and the tin which deposits as a coating component. This largely avoids fluctuations in the tin concentration in the treatment solution, which ultimately has a favorable effect on the quality, in particular the high corrosion resistance of the conversion coating.
  • the phosphate can be introduced as an alkali phosphate, such as sodium, potassium or ammonium monohydrogen phosphate or dihydrogen phosphate. It can also be formed from phosphoric acid and sodium, potassium or ammonium hydroxide. Solutions with phosphate concentrations outside the range of 1 to 50 g / l are unable to produce conversion coatings with the desired excellent properties. Concentrations within the range of 2 to 25 g / l lead to particularly high-quality conversion coatings.
  • the chlorides and / or sulfates of divalent or tetravalent tin can be used in particular as the source of tin ions.
  • Sodium stannate is also suitable.
  • the range from 0.01 to 5 g / l applies to tin II or tin IV ions, or to the sum of tin II and tin IV ions.
  • Concentrations below 0.01 g / l reduce the corrosion resistance of the conversion coatings produced.
  • concentrations above 5 g / l there is a risk that the treatment solution will become unstable. An additional improvement in the coating quality is also not achieved.
  • Complexing agents are sodium, potassium or ammonium pyrophosphate, tripolyphosphate or tetrapolyphosphate. At concentrations below 0.01 g / l, the complexing effect of the condensed phosphates is no longer sufficiently pronounced, i.e. the ability to prevent tin precipitation is waning. With concentrations above 5 g / l, an excessive pickling attack on the metal surface can be associated, in particular, the deposition of the tin in the conversion coating can be hindered.
  • phosphoric acid hydrochloric acid, sulfuric acid or sodium, potassium or ammonium hydroxide is expediently used.
  • the pH range to be set from 2 to 6 is important insofar as the corrosion resistance of the conversion coating formed becomes low at a pH value below 2 and the tendency at a pH value above 6 that tin ions precipitate out of the solution and therefore proper coating formation is no longer guaranteed.
  • the conversion coating is formed electrochemically.
  • This embodiment is particularly advantageous for the treatment of strip material made of tinplate.
  • the corrosion resistance of the conversion coating formed is particularly high.
  • the tinplate is switched as the anode against graphite, stainless steel and the like as the cathode, an electrode spacing of approximately 10 to 500 mm and a current density of approximately 0.1 A / dm 2 are set for a period of 0.5 to 60 s. Direct or alternating current can be used.
  • the conversion coating is produced in two stages, first chemically, then electrochemically. This will increase the corrosion resistance again achieved.
  • Tin-II or tin-IV and phosphate are the essential constituents forming the conversion coating.
  • the layer formation begins with the pickling attack of the acidic solution on the metal surface. It is intensified by the action of the accelerators, especially the oxo acids.
  • the complexing agent controls the tin deposition by forming a chelate complex with tin, which would otherwise easily precipitate out of the treatment solution, and provides the tin ions required for coating formation in a controlled manner.
  • Another role of the complexing agent is to bind the metal ions released from the metal surface by the pickling attack and to make them available again in a controlled manner for coating formation.
  • the complexing agent is responsible for uniform coating formation by influencing the pickling attack.
  • the coatings also have excellent properties as the basis for subsequent painting, printing and the like in terms of corrosion resistance, adhesion and gloss.
  • the treatment solution experiences practically no reduction in the tin content even after long downtimes, so that the process can then be resumed immediately and perfect conversion coatings are immediately obtained.
  • Cans made from tinplate were cleaned in a mildly alkaline cleaner with a concentration of 1% by weight in water. The coating was then sprayed for 20 s using the solutions listed below. After a water rinse, deionized water of a quality of at least 300,000 ohm ⁇ cm was sprayed for a period of 10 s and then dried in a hot air oven at 200 ° C. within 3 minutes. The conversion coating was applied in each case with a freshly prepared coating solution and one which had stood for one day for 10 cans per liter of solution.
  • H3PO4 (75% by weight) 15 g / l (PO4 11 g / l) NaClO3 6 g / l SnCl4 ⁇ 5H2O 0.6 g / l (Sn 0.2 g / l) Na4P2O7 ⁇ 10H2O 1.5 g / l (P2O7 0.6 g / l) pH 3.1 adjusted with sodium hydroxide solution
  • Tinplate cans were treated according to the procedure described in Example 1 with the following solution: H3PO4 (75% by weight) 2.8 g / l (PO4 2 g / l) NaClO3 0.3 g / l SnCl2 ⁇ 2H2O 0.04 g / l (Sn 0.02 g / l) Na4P2O7 ⁇ 10H2O 0.05 g / l (P2O7 0.02 g / l) pH 5.7 adjusted with sodium hydroxide solution Treatment temperature 70 ° C
  • tinplate cans were treated with the following solution: H3PO4 (75% by weight) 55 g / l (PO4 40 g / l) NaBrO3 17 g / l SnCl4 ⁇ 5H2O 13.2 g / l (Sn 4.5 g / l) Na5P3O10 6.5 g / l (P3O10 4.5 g / l) pH 2.2 adjusted with sodium hydroxide solution Treatment temperature 60 ° C
  • tinplate cans were treated with the following solution: H3PO4 (75% by weight) 15 g / l (PO4 11 g / l) NaClO3 6 g / l SnCl4 ⁇ 5H2O 0.6 g / l (Sn 0.2 g / l) Na4P2O7 ⁇ 10H2O 21 g / l (P2O7 8 g / l) pH 3.1 adjusted with sodium hydroxide solution Treatment temperature 60 ° C
  • the tin content was determined after the batch and after standing for one day.
  • the tinplate cans provided with conversion coatings were subjected to the corrosion test and the paint adhesion test.
  • the treated cans were immersed in tap water at 60 ° C. for 30 minutes and the rust development was assessed.
  • an epoxy / urea paint with a thickness of 5 to 7 ⁇ m was applied to the cans provided with the conversion coatings and baked at 210 ° C. (duration 10 minutes). After standing for 24 hours, the cans were immersed in a 1% by weight aqueous citric acid solution at 95 to 97 ° C and left therein for 60 minutes. It was then rinsed with water and dried.
  • the samples were provided with a cross cut reaching to the metal surface and then with cellophane adhesive tape by pressing firmly. After the adhesive tape was torn off, it was found that the paint adhesion was consistently excellent, i.e. no paint detachment was found.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Claims (4)

  1. Procédé pour appliquer des revêtements de conversion sur du fer blanc à l'aide de solutions aqueuses qui contiennent
       1 à 50 g/l d'orthophosphate (calculés pour PO₄)
       0,01 à 5 g/l d'étain
       0,2 à 20 g/l de chlorate et/ou de bromate en tant qu'accélérateur
    et un formateur de complexes,
    caractérisé en ce qu'on amène les surfaces métalliques en contact avec une solution aqueuse qui contient additionnellement
       0,01 à 5 g/l de sels de polyacides phosphoriques de formule générale : Hn+2 Pn O₃ n+1, avec n = 2, 3 ou 4 en tant que formateur de complexes
    et présente une valeur de pH de 2 à 6.
  2. Procédé selon la revendication 1,
    caractérisé en que qu'on amène les surfaces métalliques en contact avec une solution aqueuse qui contient 2 à 25 g/l d'orthophosphate.
  3. Procédé selon la revendication 1 ou 2,
    caractérisé en ce qu'on forme le revêtement de conversion par voie électrochimique.
  4. Procédé selon une ou plusieurs des revendications 1 à 3,
    caractérisé en ce qu'on forme le revêtement de conversion en deux étapes, d'abord chimiquement, ensuite électrochimiquement.
EP88202291A 1987-10-13 1988-10-13 Procédé pour produire des couches de conversion Expired - Lifetime EP0312176B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP62257678A JPH01100281A (ja) 1987-10-13 1987-10-13 金属表面の皮膜化成処理液
JP257678/87 1987-10-13

Publications (2)

Publication Number Publication Date
EP0312176A1 EP0312176A1 (fr) 1989-04-19
EP0312176B1 true EP0312176B1 (fr) 1992-12-16

Family

ID=17309584

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88202291A Expired - Lifetime EP0312176B1 (fr) 1987-10-13 1988-10-13 Procédé pour produire des couches de conversion

Country Status (10)

Country Link
US (1) US4927472A (fr)
EP (1) EP0312176B1 (fr)
JP (1) JPH01100281A (fr)
AU (1) AU608374B2 (fr)
BR (1) BR8805286A (fr)
CA (1) CA1321859C (fr)
DE (2) DE3834480A1 (fr)
GB (1) GB2210900B (fr)
MX (1) MX169760B (fr)
ZA (1) ZA887663B (fr)

Families Citing this family (28)

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AU647498B2 (en) * 1990-06-19 1994-03-24 Henkel Corporation Liquid composition and process for treating aluminium or tin cans to impart corrosion resistance and reduced friction coefficient
US5370909A (en) * 1990-06-19 1994-12-06 Henkel Corporation Liquid composition and process for treating aluminum or tin cans to impart corrosion resistance and mobility thereto
JPH04187782A (ja) * 1990-11-21 1992-07-06 Nippon Parkerizing Co Ltd ぶりきｄｉ缶用表面処理液
JPH05163584A (ja) * 1991-12-12 1993-06-29 Nippon Parkerizing Co Ltd ぶりきｄｉ缶用表面処理液
JP3256009B2 (ja) * 1992-12-09 2002-02-12 日本パーカライジング株式会社 ぶりき材表面処理液及び表面処理方法
US5498300A (en) * 1992-12-09 1996-03-12 Henkel Corporation Composition and process for treating tinplate
US5603754A (en) * 1993-07-05 1997-02-18 Henkel Corporation Composition and process for treating tinplate and aluminum
US5562950A (en) * 1994-03-24 1996-10-08 Novamax Technologies, Inc. Tin coating composition and method
JP3366724B2 (ja) * 1994-04-20 2003-01-14 日本ペイント株式会社 金属表面用化成処理水溶液
US5965205A (en) * 1995-07-21 1999-10-12 Henkel Corporation Composition and process for treating tinned surfaces
US5711996A (en) * 1995-09-28 1998-01-27 Man-Gill Chemical Company Aqueous coating compositions and coated metal surfaces
WO1998020186A1 (fr) * 1996-11-06 1998-05-14 Henkel Corporation Composition et procede de revetement par conversion a phosphate
JPH11128830A (ja) * 1997-10-30 1999-05-18 Nkk Corp 耐食性に優れた表面処理鋼板
RU2258765C2 (ru) * 2001-02-26 2005-08-20 Сумитомо Метал Индастриз, Лтд. Поверхностно-обработанный стальной материал, способ его получения и жидкость для химической конверсионной обработки
JP3873642B2 (ja) * 2001-03-21 2007-01-24 Ｊｆｅスチール株式会社 錫めっき鋼板
DE10261014B4 (de) * 2002-12-24 2005-09-08 Chemetall Gmbh Verfahren zur Beschichtung von Metalloberflächen mit einer Alkaliphosphatierungslösung, wässeriges Konzentrat und Verwendung der derart beschichteten Metalloberflächen
CN1556246A (zh) * 2004-01-08 2004-12-22 中国国际海运集装箱（集团）股份有限 无铬钝化液
KR100947947B1 (ko) * 2005-04-06 2010-03-15 렘 테크놀로지스, 인코포레이티드 고밀도 카바이드 스틸 부품의 연마 방법
DE102005023023B4 (de) * 2005-05-19 2017-02-09 Chemetall Gmbh Verfahren zur Vorbereitung von metallischen Werkstücken zum Kaltumformen, mit dem Verfahren beschichtete Werkstücke und ihre Verwendung
US20080048178A1 (en) * 2006-08-24 2008-02-28 Bruce Gardiner Aitken Tin phosphate barrier film, method, and apparatus
JP4872602B2 (ja) * 2006-10-30 2012-02-08 Ｊｆｅスチール株式会社 錫めっき鋼板の製造方法
US20080302267A1 (en) * 2007-06-05 2008-12-11 Defalco Frank G Compositions and processes for deposition of metal ions onto surfaces of conductive substrates
US8317909B2 (en) * 2007-06-05 2012-11-27 Dfhs, Llc Compositions and processes for deposition of metal ions onto surfaces of conductive substrates
US8252734B1 (en) * 2009-12-09 2012-08-28 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Friction modifier using adherent metallic multilayered or mixed element layer conversion coatings
CN103210126B (zh) * 2010-10-06 2016-09-14 塔塔钢铁艾默伊登有限责任公司 在包装钢基材上制造铁锡层的方法
DE102012212598A1 (de) * 2012-07-18 2014-02-20 Henkel Ag & Co. Kgaa Verzinnende Vorbehandlung von verzinktem Stahl in Gegenwart von Pyrophosphat
EP3872229A1 (fr) * 2020-02-28 2021-09-01 voestalpine Stahl GmbH Procédé de fabrication de composants en acier durci doté d'une couche de protection contre la corrosion en alliage de zinc conditionnée
CN114381779A (zh) * 2021-12-13 2022-04-22 首钢京唐钢铁联合有限责任公司 一种耐蚀性好的极低锡量镀锡板及其制备方法

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JPS5841352B2 (ja) * 1979-12-29 1983-09-12 日本パ−カライジング株式会社 金属表面の皮膜化成処理液
JPS60152682A (ja) * 1984-01-20 1985-08-10 Nippon Parkerizing Co Ltd りん酸塩処理方法
DE3408577A1 (de) * 1984-03-09 1985-09-12 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metallen

Also Published As

Publication number Publication date
AU2371588A (en) 1989-04-20
JPH01100281A (ja) 1989-04-18
CA1321859C (fr) 1993-09-07
BR8805286A (pt) 1989-05-30
JPH0577750B2 (fr) 1993-10-27
GB8824016D0 (en) 1988-11-23
GB2210900B (en) 1991-11-20
DE3876744D1 (de) 1993-01-28
ZA887663B (en) 1989-06-28
US4927472A (en) 1990-05-22
DE3834480A1 (de) 1989-04-27
EP0312176A1 (fr) 1989-04-19
AU608374B2 (en) 1991-03-28
GB2210900A (en) 1989-06-21
MX169760B (es) 1993-07-23

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