EP0304108B1 - Procédé de phosphatation de métaux - Google Patents
Procédé de phosphatation de métaux Download PDFInfo
- Publication number
- EP0304108B1 EP0304108B1 EP88201613A EP88201613A EP0304108B1 EP 0304108 B1 EP0304108 B1 EP 0304108B1 EP 88201613 A EP88201613 A EP 88201613A EP 88201613 A EP88201613 A EP 88201613A EP 0304108 B1 EP0304108 B1 EP 0304108B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- phosphating
- contain
- aluminum
- zinc
- fluoride
- 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
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
- C23C22/12—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 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 galvanized steel, optionally together with additionally present aluminum, as a pretreatment for the coating, which does not have the aforementioned disadvantages, but rather makes it possible to produce uniform phosphate layers on the metals which are outstanding as Are suitable for painting.
- 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 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 should 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. due to normal outdoor weathering, outdoor weathering accelerated with salt, moisture, salt spray and wash 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 table shows that flawless layers could be obtained on galvanized steel throughout the work area, with the exception of the cases in which nitrate, chloride and nickel were present in a concentration of more than 0.1 g / l each (Examples 6 and 11), insofar as the ranges essential to the invention were taken into account for the Zn, Mg and Ni concentration. Crystalline, uniform layer formation was always achieved on AlMgSi when the fluoride concentration F (el) measured electrometrically with a fluorine-sensitive electrode was in the range between 80 to 400 mg / l (Examples 4 to 6 and 13 to 20).
- 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.
Claims (5)
- Procédé pour la phosphatation d'acier zingué, éventuellement conjointement avec de l'aluminium additionnellement présent, avant la peinture avec des solutions de phosphatation à base de phosphate de magnésium et de zinc, caractérisé en ce que l'on met en contact les surfaces métalliques, à une température comprise entre 40 et 60°C, avec des solutions aqueuses de phosphatation qui contiennent
de 0,4 à 5,0 g/l de Mg
de 0,05 à 2,0 g/l de Ni
de 8 à 20 g/l de P₂O₅
et au moins un oxydant, dans lesquelles le rapport de l'acidité libre à l'acidité totale va de 0,02:1 à 0,15:1, étant entendu quea) en absence d'aluminium, la teneur en zinc des solutions de phosphatation est ajustée, dans le procédé par pistolage, à une valeur dans la plage allant de 0,4 à 1,0 g/l, et, dans le procédé par pistolage-immersion et par immersion, à une valeur dans la plage allant de 0,9 à 1,5 g/l,b) en présence d'aluminium, la teneur en zinc des solutions de phosphatation est ajustée, dans le procédé par pistolage, à une valeur dans la plage allant de 0,7 à 1,0 g/l, et, dans le procédé par pistolage-immersion et par immersion, à une valeur dans la plage allant de 1,4 à 2,0 g/l, et ces solutions ont en outre une teneur en fluorure ["F(el)", déterminée au moyen d'une électrode sensible aux fluorures, immergée dans la solution de bain] allant de 80 à 400 mg/l. - Procédé selon la revendication 1, caractérisé en ce que l'on met en contact les surfaces métalliques avec des solutions de phosphatation qui contiennent, en tant qu'oxydant, un nitrate, un nitrite, un chlorate, un bromate, un peroxyde et/ou un nitrobenzènesulfonate.
- Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on met en contact les surfaces métalliques avec des solutions de phosphatation qui contiennent, parmi les trois composants (chlorure et/ou bromure), (nitrate) et (nickel), au moins un composant à une concentration n'excédant pas 0,1 g/l.
- Procédé selon la revendication 1, 2 ou 3, caractérisé en ce que l'on met en contact les surfaces métalliques avec des solutions de phosphatation qui contiennent un fluorure simple ou complexe.
- Procédé selon une ou plusieurs des revendications 1 à 5, caractérisé en ce que les pièces phosphatées sont ensuite peintes par trempage électrophorétique, de préférence peintes par immersion dans un bain de cataphorèse.
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 EP0304108A1 (fr) | 1989-02-22 |
EP0304108B1 true 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) |
Families Citing this family (25)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3828676A1 (de) * | 1988-08-24 | 1990-03-01 | Metallgesellschaft Ag | Phosphatierverfahren |
JPH03107469A (ja) * | 1989-09-21 | 1991-05-07 | Nippon Parkerizing Co Ltd | 裸耐食性に優れたりん酸塩化成皮膜を有する亜鉛系めっき材料 |
KR100197145B1 (ko) * | 1989-12-19 | 1999-06-15 | 후지이 히로시 | 금속표면의 인산아연 처리방법 |
JP2695963B2 (ja) * | 1990-03-16 | 1998-01-14 | マツダ株式会社 | 金属表面のリン酸塩処理方法 |
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 |
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 |
JP3181658B2 (ja) * | 1992-01-13 | 2001-07-03 | 日本パーカライジング株式会社 | 金属材料の酸性化成処理における有効フッ素濃度の定量方法 |
JPH05306497A (ja) | 1992-04-30 | 1993-11-19 | Nippondenso Co Ltd | リン酸塩化成処理方法 |
DE4306446A1 (de) * | 1993-03-02 | 1994-09-08 | Metallgesellschaft Ag | Verfahren zur Erleichterung der Kaltumformung |
JPH07173643A (ja) * | 1993-12-21 | 1995-07-11 | Mazda Motor Corp | 金属表面の燐酸塩処理方法及び処理液 |
US5478413A (en) * | 1994-12-27 | 1995-12-26 | Sermatech International, Inc. | Environmentally friendly coating compositions |
US5797987A (en) * | 1995-12-14 | 1998-08-25 | Ppg Industries, Inc. | Zinc phosphate conversion coating compositions and process |
DE19606018A1 (de) * | 1996-02-19 | 1997-08-21 | Henkel Kgaa | Zinkphosphatierung mit geringen Gehalten an Nickel- und/oder Cobalt |
US6413588B1 (en) | 1999-01-11 | 2002-07-02 | E. I. Du Pont De Nemours And Company | Method of producing durable layered coatings |
DE19921135A1 (de) * | 1999-05-07 | 2000-11-09 | Henkel Kgaa | Verfahren zur nickelarmen Zinkphoshatierung mit anschließender Wasserbehandlung |
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 |
DE102005059314B4 (de) * | 2005-12-09 | 2018-11-22 | Henkel Ag & Co. Kgaa | Saure, chromfreie wässrige Lösung, deren Konzentrat, und ein Verfahren zur Korrosionsschutzbehandlung von Metalloberflächen |
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 |
KR101106516B1 (ko) | 2006-10-31 | 2012-01-20 | 제이에프이 스틸 가부시키가이샤 | 인산염 처리 아연계 도금 강판 및 그 제조 방법 |
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 |
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. |
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 |
KR101830508B1 (ko) * | 2016-06-24 | 2018-02-21 | 주식회사 포스코 | 내변색성 및 필름 접착성이 우수한 인산염 처리 아연계 도금강판 |
Family Cites Families (11)
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 |
US3597283A (en) * | 1969-10-08 | 1971-08-03 | Lubrizol Corp | Phosphating solutions for use on ferrous metal and zinc surfaces |
US3676224A (en) * | 1970-10-16 | 1972-07-11 | Lubrizol Corp | Phosphating solution with scale suppressing characteristics |
DE2327304C3 (de) * | 1973-05-29 | 1982-01-21 | Metallgesellschaft Ag, 6000 Frankfurt | Verfahren zum Aufbringen von Phosphatüberzügen auf Metalle |
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 |
EP0172806A4 (fr) * | 1984-01-06 | 1986-05-16 | Ford Motor Co | Revetement de conversion de phosphate a resistance alcaline. |
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 |
DE3630246A1 (de) * | 1986-09-05 | 1988-03-10 | Metallgesellschaft Ag | Verfahren zur erzeugung von phosphatueberzuegen sowie dessen anwendung |
-
1988
- 1988-07-26 ES ES198888201613T patent/ES2036666T3/es not_active Expired - Lifetime
- 1988-07-26 DE DE8888201613T patent/DE3871031D1/de not_active Expired - Lifetime
- 1988-07-26 EP EP88201613A patent/EP0304108B1/fr not_active Expired - Lifetime
- 1988-08-09 CA CA000574254A patent/CA1333147C/fr not_active Expired - Fee Related
- 1988-08-12 JP JP63200322A patent/JP2680618B2/ja not_active Expired - Lifetime
- 1988-08-19 GB GB8819791A patent/GB2208876B/en not_active Expired - Lifetime
- 1988-08-19 ZA ZA886167A patent/ZA886167B/xx unknown
Also Published As
Publication number | Publication date |
---|---|
GB2208876A (en) | 1989-04-19 |
GB2208876B (en) | 1991-08-14 |
DE3871031D1 (de) | 1992-06-17 |
ES2036666T3 (es) | 1993-06-01 |
EP0304108A1 (fr) | 1989-02-22 |
JP2680618B2 (ja) | 1997-11-19 |
CA1333147C (fr) | 1994-11-22 |
GB8819791D0 (en) | 1988-09-21 |
ZA886167B (en) | 1990-04-25 |
JPS6468481A (en) | 1989-03-14 |
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