EP0304108A1 - Procédé de phosphatation de métaux - Google Patents

Procédé de phosphatation de métaux Download PDF

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Publication number
EP0304108A1
EP0304108A1 EP88201613A EP88201613A EP0304108A1 EP 0304108 A1 EP0304108 A1 EP 0304108A1 EP 88201613 A EP88201613 A EP 88201613A EP 88201613 A EP88201613 A EP 88201613A EP 0304108 A1 EP0304108 A1 EP 0304108A1
Authority
EP
European Patent Office
Prior art keywords
phosphating
value
phosphating solutions
range
spray
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.)
Granted
Application number
EP88201613A
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German (de)
English (en)
Other versions
EP0304108B1 (fr
Inventor
Werner Dr. Rausch
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
Original Assignee
Metallgesellschaft AG
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 filed Critical Metallgesellschaft AG
Publication of EP0304108A1 publication Critical patent/EP0304108A1/fr
Application granted granted Critical
Publication of EP0304108B1 publication Critical patent/EP0304108B1/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
    • C23C22/12—Orthophosphates containing 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
    • C23C22/368—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 and / or galvanized steel, optionally together with additionally present aluminum, before painting with phosphating solutions based on zinc magnesium phosphate.
  • the object of the invention is to provide a process for the phosphating of steel and / or galvanized steel, optionally together with additionally present aluminum, as a pretreatment for the coating, which does not have the aforementioned disadvantages, but rather enables uniform phosphate layers to be produced on the metals , which are excellent as a basis for painting.
  • the method according to the invention is suitable for the phosphating of all unalloyed and low-alloy steels.
  • galvanized steel is understood to mean steel which, for example, on the hot-dip path or in the electrolytic process with zinc or zinc alloy coatings e.g. Pure zinc, zinc nickel, zinc iron, zinc aluminum was coated.
  • zinc or zinc alloy coatings e.g. Pure zinc, zinc nickel, zinc iron, zinc aluminum was coated.
  • aluminum in the sense of the invention includes Pure aluminum and alloys of aluminum with magnesium, zinc, copper, silicon, manganese etc.
  • the concentration of fluoride detected with the fluoride-sensitive electrode corresponds approximately to that in the Phosphating solution present proportion of dissociated fluoride (F ⁇ ).
  • F (el) value 80 to 400 mg / l at the usual phosphating bath pH values of the baths, about 0.4 to 0.9 g / l NH4HF2 or equivalent amounts of other single fluoride-containing compounds must be added will.
  • the bath is preferably supplemented by adding enough fluoride-containing compound to the phosphating bath until the desired measured value of F (el) is reached.
  • the metal surfaces to be treated must be free from disruptive deposits of oils, lubricants, oxides and the like, which can impair proper layer formation.
  • the surfaces are cleaned in a suitable manner.
  • the surface is preferably coated with an activating agent known per se, e.g. an aqueous suspension containing titanium phosphate, activated.
  • the activating agent can be used in the cleaning bath or as a separate process step.
  • the phosphating solutions according to the invention are used in spraying, spray-immersion or immersion at temperatures between 40 and 60 ° C.
  • the times during which the metal surfaces are brought into contact with the phosphating solution to form a covering phosphate layer are in the case of galvanized steel, e.g. between 20 sec and 10 min, for steel and aluminum e.g. between 1 and 10 min.
  • the cations zinc, magnesium and nickel are in the Phosphating solution introduced, for example, as metal, oxide, carbonate, phosphate, nitrate, chloride and / or complex fluoride.
  • the phosphate portion is fed to the solution via phosphates and / or phosphoric acid.
  • additional cations for example Na, K, NH4 or anions, for example nitrate, chloride, sulfate, are used.
  • the value of the free acid (total acid) is identical to the consumption of ml 0.1 n NaOH for neutralizing a 10 ml bath sample against the first turning point (second turning point) of the phosphoric acid.
  • the phosphating bath also contains at least one oxidizing agent from the group consisting of nitrate, nitrite, chlorate, bromate, peroxide and nitrobene sulfonate, e.g. the following quantities can be used: 2 to 20 g / l nitrate; 0.05 to 0.5 g / l nitrite; 0.5 to 5 g / l chlorate; 0.2 to 3 g / l bromate; 0.02 to 0.1 g / l peroxide; 0.1 to 1 g / l nitrobenzenesulfonate.
  • the oxidizing agents can also be combined with one another, e.g. Nitrate nitrite, (nitrate) chlorate nitrite, nitrate bromate, (nitrate) chlorate nitrobenzenesulfonate, nitrate nitrobenzenesulfonate.
  • the three components chloride and / or Bromide), (nitrate) and (nickel) only two each in a concentration of more than 0.1 g / l, while the third may only be present in a maximum concentration of 0.1 g / l.
  • Chloride and bromide are counted as one component and their individual concentrations are added. Chloride can, for example, get into the phosphating bath from the preparation water for the phosphating solution and / or as a reduction product of chlorate.
  • the bromate accelerator in particular is to be regarded as the source.
  • the phosphating bath preferably contains simple and / or complex fluoride.
  • the group of suitable complex fluorides includes e.g. Fluoroborates and fluorosilicates.
  • the phosphating solutions used in the process according to the invention can also contain further additives, but mostly in minor amounts. These include Copper, manganese, calcium, iron, cobalt, polyphosphates, polyhydroxycarboxylic acids, surfactants and agents for influencing the sludge separation.
  • the phosphate layers produced according to the invention are used as preparation for a subsequent painting. They are preferably used for workpieces which are subsequently electrocoated, in particular cathodically electrocoated. In this way you get layers of paint, which are characterized by a high resistance to infiltration when exposed to corrosion, e.g. normal outdoor weathering, outdoor weathering accelerated with salt, moisture, salt spray and washing liquor and have very good adhesion to scratching and impact stress before and after corrosion.
  • the method according to the invention is particularly suitable for the pretreatment of housings for household appliances and technical apparatus, of metal furniture, of vehicle bodies and of vehicle accessories before painting.
  • Sheets made of steel, electrolytically galvanized steel, hot-dip galvanized steel and AlMgSi were treated after alkaline cleaning, water rinsing and activation in an aqueous titanium phosphate suspension with the phosphating solutions listed in the table at 50 ° C for 2 minutes by spraying or 3 minutes by immersion. This was followed by rinsing with water, an aqueous passivating solution containing chromium (VI), demineralized water and a drying stage.
  • VI chromium
  • the layers were provided with a cathodic electrodeposition paint and an automotive paint structure and subjected to the usual technical tests. In all cases where crystalline layers were present on the metal substrate, excellent test results were achieved.

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)
EP88201613A 1987-08-19 1988-07-26 Procédé de phosphatation de métaux Expired - Lifetime EP0304108B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3727613 1987-08-19
DE3727613 1987-08-19

Publications (2)

Publication Number Publication Date
EP0304108A1 true EP0304108A1 (fr) 1989-02-22
EP0304108B1 EP0304108B1 (fr) 1992-05-13

Family

ID=6334038

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88201613A Expired - Lifetime EP0304108B1 (fr) 1987-08-19 1988-07-26 Procédé de phosphatation de métaux

Country Status (7)

Country Link
EP (1) EP0304108B1 (fr)
JP (1) JP2680618B2 (fr)
CA (1) CA1333147C (fr)
DE (1) DE3871031D1 (fr)
ES (1) ES2036666T3 (fr)
GB (1) GB2208876B (fr)
ZA (1) ZA886167B (fr)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991004354A1 (fr) * 1989-09-21 1991-04-04 Henkel Corporation Articles a surfaces zinciferes presentant une resistance a la corrosion avant peinture amelioree, et leurs procedes de fabrication et d'utilisation
EP0434358A2 (fr) * 1989-12-19 1991-06-26 Nippon Paint Co., Ltd. Procédé de phosphatation au phosphate de zinc de surfaces métalliques
EP0452638A1 (fr) * 1990-03-16 1991-10-23 Mazda Motor Corporation Méthode de traitement pour la phosphatation de surfaces métalliques
WO1993014241A1 (fr) * 1992-01-13 1993-07-22 Henkel Corporation Procede de traitement par conversion acide d'un metal contenant de l'aluminium
EP0613964A1 (fr) * 1993-03-02 1994-09-07 Metallgesellschaft Aktiengesellschaft Procédé facilitant la déformation à froid
EP0659906A1 (fr) * 1993-12-21 1995-06-28 Mazda Motor Corporation Procédé et solution de phosphatation de surfaces métalliques
US5454882A (en) * 1992-01-13 1995-10-03 Henkel Corporation Process for controlling a fluoride containing conversion coating forming composition during its use for conversion coating aluminum containing metal
WO1997021850A1 (fr) * 1995-12-14 1997-06-19 Ppg Industries, Inc. Compositions pour revetement de conversion en phosphate de zinc et procede afferent
WO1997030189A1 (fr) * 1996-02-19 1997-08-21 Henkel Kommanditgesellschaft Auf Aktien Procede de phosphatisation au zinc a l'aide de faibles teneurs en nickel et/ou en cobalt
EP0728851B1 (fr) * 1994-12-27 2000-03-15 Sermatech International Inc. Composition de revêtement respectant l'environnement
WO2000068154A1 (fr) * 1999-05-07 2000-11-16 Henkel Kommanditgesellschaft Auf Aktien Procede de phosphatation au zinc au moyen d'une solution a faible teneur en nickel et traitement consecutif des eaux usees
CN102430506A (zh) * 2011-12-15 2012-05-02 江苏腾奇电力设备科技有限公司 用于散热器铸件的涂漆工艺
EP2767615A1 (fr) * 2005-12-09 2014-08-20 Henkel AG&Co. KGAA Procédé au trempé et solution acide sans chrome destinés au traitement anticorrosion de surfaces en aciers

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3828676A1 (de) * 1988-08-24 1990-03-01 Metallgesellschaft Ag Phosphatierverfahren
DE4131382A1 (de) * 1990-09-21 1992-03-26 Kobe Steel Ltd Oberflaechenbehandeltes aluminiumlegierungsblech fuer den automobilbau und verfahren zu dessen herstellung
US5144611A (en) * 1990-10-01 1992-09-01 International Business Machines Corporation Optical disk drive cleaner cartridge
JPH05306497A (ja) 1992-04-30 1993-11-19 Nippondenso Co Ltd リン酸塩化成処理方法
US6413588B1 (en) 1999-01-11 2002-07-02 E. I. Du Pont De Nemours And Company Method of producing durable layered coatings
JP4658339B2 (ja) * 2001-01-17 2011-03-23 日本ペイント株式会社 金属表面処理方法
JP5119864B2 (ja) * 2006-10-31 2013-01-16 Ｊｆｅスチール株式会社 リン酸塩処理亜鉛系めっき鋼板及びその製造方法
SG176435A1 (en) 2006-10-31 2011-12-29 Jfe Steel Corp Phosphate-treated galvanized steel sheet and method for making the same
JP4992385B2 (ja) * 2006-10-31 2012-08-08 Ｊｆｅスチール株式会社 有機樹脂被覆リン酸塩処理亜鉛系めっき鋼板及びその製造方法
JP2007314888A (ja) * 2007-07-17 2007-12-06 Toyota Motor Corp 多層塗膜構造
ES2397997B1 (es) * 2010-03-22 2014-01-17 Roberto Ruiz Sanz Depósito by pass para aire comprimido.
KR101830508B1 (ko) * 2016-06-24 2018-02-21 주식회사 포스코 내변색성 및 필름 접착성이 우수한 인산염 처리 아연계 도금강판

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2049350A1 (de) * 1969-10-08 1971-04-15 Lubrizol Corp Phosphatierungslosungen und ihre Verwendung zum Korrosionsschutz von Eisen metall und Zinkoberflachen
FR2111665A1 (fr) * 1970-10-16 1972-06-09 Lubrizol Corp
FR2231775A1 (en) * 1973-05-29 1974-12-27 Parker Ste Continentale Phosphate-coating solns. - free from formation of water-soluble salts during neutralization
WO1985003089A1 (fr) * 1984-01-06 1985-07-18 Ford Motor Company Revetement de conversion de phosphate a resistance alcaline
EP0258922A1 (fr) * 1986-09-05 1988-03-09 Metallgesellschaft Ag Procédé pour produire des revêtements de phosphate et leur utilisation

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB648888A (en) * 1947-04-25 1951-01-17 Walterisation Company Ltd Improvements in the production of phosphate coatings on metal surfaces
JPS5165041A (en) * 1974-12-04 1976-06-05 Nippon Packaging Kk Kinzokuno rinsanenhimakukeiseihoho
US4529451A (en) * 1983-01-03 1985-07-16 Detrex Chemical Industries, Inc. Zinc phosphate coated metal and process of producing same
DE3311738A1 (de) * 1983-03-31 1984-10-04 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metalloberflaechen
DE3408577A1 (de) * 1984-03-09 1985-09-12 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metallen
US4595424A (en) * 1985-08-26 1986-06-17 Parker Chemical Company Method of forming phosphate coating on zinc

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2049350A1 (de) * 1969-10-08 1971-04-15 Lubrizol Corp Phosphatierungslosungen und ihre Verwendung zum Korrosionsschutz von Eisen metall und Zinkoberflachen
FR2111665A1 (fr) * 1970-10-16 1972-06-09 Lubrizol Corp
FR2231775A1 (en) * 1973-05-29 1974-12-27 Parker Ste Continentale Phosphate-coating solns. - free from formation of water-soluble salts during neutralization
WO1985003089A1 (fr) * 1984-01-06 1985-07-18 Ford Motor Company Revetement de conversion de phosphate a resistance alcaline
EP0258922A1 (fr) * 1986-09-05 1988-03-09 Metallgesellschaft Ag Procédé pour produire des revêtements de phosphate et leur utilisation

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991004354A1 (fr) * 1989-09-21 1991-04-04 Henkel Corporation Articles a surfaces zinciferes presentant une resistance a la corrosion avant peinture amelioree, et leurs procedes de fabrication et d'utilisation
EP0434358A2 (fr) * 1989-12-19 1991-06-26 Nippon Paint Co., Ltd. Procédé de phosphatation au phosphate de zinc de surfaces métalliques
EP0434358A3 (en) * 1989-12-19 1992-10-28 Nippon Paint Co., Ltd. Method for phosphating metal surface with zinc phosphate
US5399208A (en) * 1989-12-19 1995-03-21 Nippon Paint Co., Ltd. Method for phosphating metal surface with zinc phosphate
EP0452638A1 (fr) * 1990-03-16 1991-10-23 Mazda Motor Corporation Méthode de traitement pour la phosphatation de surfaces métalliques
WO1993014241A1 (fr) * 1992-01-13 1993-07-22 Henkel Corporation Procede de traitement par conversion acide d'un metal contenant de l'aluminium
US5454882A (en) * 1992-01-13 1995-10-03 Henkel Corporation Process for controlling a fluoride containing conversion coating forming composition during its use for conversion coating aluminum containing metal
EP0613964A1 (fr) * 1993-03-02 1994-09-07 Metallgesellschaft Aktiengesellschaft Procédé facilitant la déformation à froid
US5415701A (en) * 1993-03-02 1995-05-16 Metallgesellschaft Aktiengesellschaft Process for facilitating cold-working operations
CN1040779C (zh) * 1993-03-02 1998-11-18 金属股份公司 便于冷加工操作的方法
US5536336A (en) * 1993-12-21 1996-07-16 Nippon Paint Co., Ltd. Method of phosphating metal surfaces and treatment solution
EP0659906A1 (fr) * 1993-12-21 1995-06-28 Mazda Motor Corporation Procédé et solution de phosphatation de surfaces métalliques
EP0728851B1 (fr) * 1994-12-27 2000-03-15 Sermatech International Inc. Composition de revêtement respectant l'environnement
WO1997021850A1 (fr) * 1995-12-14 1997-06-19 Ppg Industries, Inc. Compositions pour revetement de conversion en phosphate de zinc et procede afferent
US5797987A (en) * 1995-12-14 1998-08-25 Ppg Industries, Inc. Zinc phosphate conversion coating compositions and process
US5868874A (en) * 1995-12-14 1999-02-09 Ppg Industries, Inc. Zinc phosphate conversion coating compositions and process
WO1997030189A1 (fr) * 1996-02-19 1997-08-21 Henkel Kommanditgesellschaft Auf Aktien Procede de phosphatisation au zinc a l'aide de faibles teneurs en nickel et/ou en cobalt
WO2000068154A1 (fr) * 1999-05-07 2000-11-16 Henkel Kommanditgesellschaft Auf Aktien Procede de phosphatation au zinc au moyen d'une solution a faible teneur en nickel et traitement consecutif des eaux usees
EP2767615A1 (fr) * 2005-12-09 2014-08-20 Henkel AG&Co. KGAA Procédé au trempé et solution acide sans chrome destinés au traitement anticorrosion de surfaces en aciers
CN102430506A (zh) * 2011-12-15 2012-05-02 江苏腾奇电力设备科技有限公司 用于散热器铸件的涂漆工艺

Also Published As

Publication number Publication date
ES2036666T3 (es) 1993-06-01
CA1333147C (fr) 1994-11-22
ZA886167B (en) 1990-04-25
GB8819791D0 (en) 1988-09-21
EP0304108B1 (fr) 1992-05-13
JPS6468481A (en) 1989-03-14
GB2208876B (en) 1991-08-14
JP2680618B2 (ja) 1997-11-19
GB2208876A (en) 1989-04-19
DE3871031D1 (de) 1992-06-17

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