EP0454211B1 - Verfahren zum Aufbringen von Phosphatüberzügen auf Metalloberflächen - Google Patents
Verfahren zum Aufbringen von Phosphatüberzügen auf Metalloberflächen Download PDFInfo
- Publication number
- EP0454211B1 EP0454211B1 EP91200844A EP91200844A EP0454211B1 EP 0454211 B1 EP0454211 B1 EP 0454211B1 EP 91200844 A EP91200844 A EP 91200844A EP 91200844 A EP91200844 A EP 91200844A EP 0454211 B1 EP0454211 B1 EP 0454211B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- activating
- phosphate
- copper
- steel
- quantities
- 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
- C23C22/78—Pretreatment of the material to be coated
- C23C22/80—Pretreatment of the material to be coated with solutions containing titanium or zirconium compounds
Definitions
- the invention relates to a method for applying phosphate coatings on metal surfaces by activation with an activating agent based on Ti IV phosphate and zinc phosphating.
- zinc phosphate layers can be produced on numerous metallic surfaces, such as iron, steel, galvanized alloy steel, aluminum or aluminized steel.
- the zinc phosphate layers obtained serve to protect against corrosion, paint adhesion, reduction of sliding resistance, ease of cold forming and electrical insulation.
- a phosphating process also includes various pre-treatment and post-treatment stages. It is essential to clean the metal surface, which is generally done with alkaline or acidic cleaners and removes oils, greases, oxides and adhering solid particles from the metal surface. If cleaning is carried out with mildly alkaline cleaners, it is in principle possible to combine cleaning with activation of the metal surface. As a rule, however, the activation follows the cleaning as a separate process step.
- the task of activating the metal surface is to form a with the shortest possible phosphating times to ensure the finest possible crystalline zinc phosphate layer.
- a criterion for the effectiveness of an activating agent is therefore the minimum phosphating time.
- the suitability for forming even finely crystalline zinc phosphate layers can be determined on the basis of the layer weights or by scanning electron microscope images.
- Titan IV phosphates form when aqueous titanium IV salt solutions are reacted with soluble phosphates or phosphoric acid.
- products with activating properties are only obtained under special manufacturing conditions, which are described, for example, in US Pat. Nos. 2,310,239 and 2,456,947 and provide precise information regarding the type and concentration of the raw materials, temperature and pH range during manufacture.
- the reaction conditions are kept constant, there are fluctuations in the application effect from batch to batch.
- activation agents based on titanium IV phosphate have to be prepared with deionized water.
- the reason for this is that the alkaline earth metal ions present in the tap water as hardening agents destabilize titanium IV phosphate in activation baths.
- These alkaline earth metal ions can also be introduced into the activation bath by rinsing water.
- DE-A-3731089 proposes that cation-exchanging zeolites with a primary particle diameter of ⁇ 3 »m the activating one Mix in titanium phosphate.
- Another way to improve the activation baths is described in EP-B-180523.
- the addition of phosphonic acid acting as a complexing agent into the activation bath permits the use of industrial water for the bath preparation.
- the phosphonic acid is said to cause the zinc phosphate layer to become extremely fine crystalline.
- a serious disadvantage of individual phosphonic acids is that they act as a phosphating bath poison even in concentrations of a few mg / l. An entry of phosphonic acid from the activation bath into the phosphating bath can render the phosphating bath unusable in a very short time.
- DE-A-3814287 provides for poly (aldehyde carboxylic acids) to be added in substoichiometric amounts as complexing agents for titanium IV during the production of activating titanium IV phosphates.
- the introduction of the poly (aldehyde carboxylic acids) into the phosphating bath can have considerable disadvantages.
- Activating agents based on Ti IV phosphate containing at least one of the divalent metals barium, strontium and calcium are also known (FR-A-2 114 874).
- the number of equivalents of titanium should not exceed the number of equivalents of divalent metals.
- the result of the activating cleaning prior to zinc phosphating is reported using cleaning liquids which have a pH greater than 12 and which contain, inter alia, an activating agent based on Ti IV phosphate modified with a copper compound. According to the presentation in FR-A-2 114 874, this pretreatment leads to thin, powdery, irregular phosphate layers with coarse crystals in the subsequent zinc phosphating.
- the object of the invention is to provide a method for applying phosphate coatings on metal surfaces by activation with an activating agent based on Ti IV phosphate and zinc phosphating, which does not have the disadvantages of the known processes, provides for the use of an activating agent which is simple to produce and for stable activation baths with a long service life, which also guarantee the formation of fine crystalline zinc phosphate layers in a short time.
- the object is achieved by designing the method of the type mentioned at the outset in accordance with the invention in such a way that the metal surfaces are activated with an activation bath which 0.001 to 0.060 g / l Ti 0.020 to 1.2 g / l orthophosphate (calc. As P2O5) and 0.001 to 0.1 g / l Cu and contains so much alkali that it has a pH of 7 to 11.
- an activation bath which 0.001 to 0.060 g / l Ti 0.020 to 1.2 g / l orthophosphate (calc. As P2O5) and 0.001 to 0.1 g / l Cu and contains so much alkali that it has a pH of 7 to 11.
- the copper content was adjusted by adding copper compounds. These compounds have the effect that the minimum phosphating time is reduced considerably.
- the addition of copper also means that the activation bath is stable over a wide temperature range and shows very good activating properties.
- the activating agent contains copper compounds introduced via copper hydroxide, copper oxide hydrate, copper tartrate, copper nitrate and / or copper phosphate. Copper sulfate or copper chloride can be used but are not preferred.
- Copper concentrations above 0.1 g / l should be avoided since they can lead to a disruption in the phosphating in the subsequent step.
- activating agent was produced which corresponded to activating agent 2 in terms of composition, but did not contain any copper phosphate.
- Activating agent 1 was used as activating agent 3, to which maleic anhydride copolymer was added in such a way that the resulting activating bath contained 10 mg / l.
- Activating agent 1 which was mixed with surfactant in such quantities that the surfactant concentration of 0.3 g / l was formed when the activation bath was prepared, also served as the starting product.
- the degree of layer coverage was determined in percent. This value indicates the proportion of the metal surface that is provided with a closed zinc phosphate layer.
- the assessment was made visually.
- the layer weight of the phosphate coating was determined gravimetrically and the minimum phosphating times determined.
- the minimum phosphating time is the minimum time required to form a closed phosphate layer.
- the crystallinity of the phosphate layers was checked using scanning electron microscope images at a magnification of 2000 times.
- the activating agent according to Examples 1, 2, 3 and 4 leads to a high, almost complete coverage of the metal surface after just 3 minutes of phosphating or enables short treatment times in the subsequent phosphating step.
- the weight of the phosphate layer is well within the usual range.
- the results for the activating agents 3 and 4 indicate that the addition of maleic anhydride copolymer or surfactant leads to a considerable increase in the service life of the activating bath if the short minimum phosphating time is observed (cf. activating agent 1).
- the investigations with the scanning electron microscope showed that the phosphate layers obtained using the activating agents 1, 2, 3 and 4 were of fine-grained nature.
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- 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)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Materials For Medical Uses (AREA)
- Detergent Compositions (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4012795 | 1990-04-21 | ||
DE4012795A DE4012795A1 (de) | 1990-04-21 | 1990-04-21 | Aktivierungsmittel fuer die phosphatierung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0454211A1 EP0454211A1 (de) | 1991-10-30 |
EP0454211B1 true EP0454211B1 (de) | 1994-06-22 |
Family
ID=6404842
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP91200844A Expired - Lifetime EP0454211B1 (de) | 1990-04-21 | 1991-04-11 | Verfahren zum Aufbringen von Phosphatüberzügen auf Metalloberflächen |
Country Status (9)
Country | Link |
---|---|
US (1) | US5160551A (ja) |
EP (1) | EP0454211B1 (ja) |
JP (1) | JP3063921B2 (ja) |
AT (1) | ATE107711T1 (ja) |
BR (1) | BR9101616A (ja) |
CA (2) | CA2040859C (ja) |
DE (2) | DE4012795A1 (ja) |
ES (1) | ES2055518T3 (ja) |
ZA (1) | ZA912943B (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102008054407A1 (de) | 2008-12-09 | 2010-06-10 | Chemetall Gmbh | Verfahren zur Beschichtung von metallischen Oberflächen mit einem Aktivierungsmittel vor dem Phosphatieren |
DE102018216216A1 (de) * | 2018-09-24 | 2020-03-26 | Thyssenkrupp Ag | Verfahren zur Verbesserung der Phosphatierbarkeit von metallischen Oberflächen, welche mit einer temporären Vor- bzw. Nachbehandlung versehen werden |
DE102019134298A1 (de) * | 2019-12-13 | 2021-06-17 | Thyssenkrupp Steel Europe Ag | Verfahren zum Herstellen eines Stahlflachprodukts mit einer metallischen Schutzschicht auf Basis von Zink und einer auf einer Oberfläche der metallischen Schutzschicht erzeugten Phosphatierschicht und derartiges Stahlflachprodukt |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2686622B1 (fr) * | 1992-01-29 | 1995-02-24 | Francais Prod Ind Cfpi | Concentre pour bain d'activation et d'affinage et bain obtenu a partir de ce concentre. |
US5628838A (en) * | 1992-01-29 | 1997-05-13 | C.F.P.I Societe Anonyme | Concentrate for activating and defining bath and bath obtained from this concentrate |
DE4232292A1 (de) * | 1992-09-28 | 1994-03-31 | Henkel Kgaa | Verfahren zum Phosphatieren von verzinkten Stahloberflächen |
DE4416619A1 (de) * | 1994-05-11 | 1995-11-16 | Henkel Kgaa | Herstellung phosphathaltiger Aktiviermittel für die Phosphatierung unter Einsatz von Mikrowellen |
US5494504A (en) * | 1994-09-12 | 1996-02-27 | Ppg Industries, Inc. | Liquid rinse conditioner for phosphate conversion coatings |
JP3451334B2 (ja) * | 1997-03-07 | 2003-09-29 | 日本パーカライジング株式会社 | 金属のりん酸塩皮膜化成処理前の表面調整用前処理液及び表面調整方法 |
MY129412A (en) * | 1998-07-21 | 2007-03-30 | Nihon Parkerizing | Conditioning liquid and conditioning process used in pretreatment for formation of phosphate layer on the metallic surface |
JP2007204835A (ja) * | 2006-02-03 | 2007-08-16 | Nippon Paint Co Ltd | 表面調整用組成物及び表面調整方法 |
DE102008047533A1 (de) | 2008-09-16 | 2010-04-15 | Sachtleben Chemie Gmbh | Verfahren zur Herstellung von Titan-IV-phosphat |
DE102011051879B4 (de) | 2011-07-15 | 2023-11-09 | Dürr Systems Ag | Anlage und Verfahren zur Oberflächenbehandlung von Werkstücken sowie Verwendung einer solchen Anlage zum Lackieren von Werkstücken |
DE102013202286B3 (de) | 2013-02-13 | 2014-01-30 | Chemetall Gmbh | Verwendung eines Silan-, Silanol- oder/und Siloxan-Zusatzes zur Vermeidung von Stippen auf Zink-haltigen Metalloberflächen und Verwendung der beschichteten Metallsubstrate |
CN103741132B (zh) * | 2014-01-10 | 2016-08-17 | 湖南金裕化工有限公司 | 胶钛表面调整剂及其制备方法 |
DE102014105226A1 (de) | 2014-04-11 | 2015-10-15 | Thyssenkrupp Ag | Verfahren zur Aktivierung von zu phosphatierenden Metalloberflächen, vorzugsweise verzinktem Stahlblech |
KR20200045487A (ko) * | 2017-08-31 | 2020-05-04 | 케메탈 게엠베하 | 금속 표면을 니켈-무함유 인산염처리하는 개선된 방법 |
CN114990537B (zh) * | 2022-08-04 | 2022-11-25 | 山东一立动力科技股份有限公司 | 一种铝合金表面磷化处理方法 |
EP4339324A1 (de) * | 2022-09-19 | 2024-03-20 | ThyssenKrupp Steel Europe AG | Stahlflachprodukt mit einer aktivierungsschicht für die warmumformung |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE410815A (ja) * | 1934-08-13 | |||
US2329065A (en) * | 1942-03-06 | 1943-09-07 | Westinghouse Electric & Mfg Co | Corrosion resistant coating for metal surfaces |
US3166444A (en) * | 1962-04-26 | 1965-01-19 | Lubrizol Corp | Method for cleaning metal articles |
CA960944A (en) * | 1970-11-19 | 1975-01-14 | Dulux Australia Ltd. | Grain-refining compounds |
JPS5591997A (en) * | 1978-12-30 | 1980-07-11 | Nippon Parkerizing Co Ltd | Surface treating method of steel plate |
DE3814363A1 (de) * | 1988-04-28 | 1989-11-09 | Henkel Kgaa | Titanfreie aktivierungsmittel, verfahren zu ihrer herstellung und ihre verwendung zur aktivierung von metalloberflaechen vor einer zinkphosphatierung |
-
1990
- 1990-04-21 DE DE4012795A patent/DE4012795A1/de not_active Withdrawn
-
1991
- 1991-04-11 DE DE59101978T patent/DE59101978D1/de not_active Expired - Fee Related
- 1991-04-11 ES ES91200844T patent/ES2055518T3/es not_active Expired - Lifetime
- 1991-04-11 EP EP91200844A patent/EP0454211B1/de not_active Expired - Lifetime
- 1991-04-11 AT AT91200844T patent/ATE107711T1/de not_active IP Right Cessation
- 1991-04-17 US US07/686,825 patent/US5160551A/en not_active Expired - Lifetime
- 1991-04-19 CA CA002040859A patent/CA2040859C/en not_active Expired - Fee Related
- 1991-04-19 CA CA002040872A patent/CA2040872A1/en not_active Abandoned
- 1991-04-19 ZA ZA912943A patent/ZA912943B/xx unknown
- 1991-04-22 BR BR919101616A patent/BR9101616A/pt unknown
- 1991-04-22 JP JP3118013A patent/JP3063921B2/ja not_active Expired - Fee Related
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102008054407A1 (de) | 2008-12-09 | 2010-06-10 | Chemetall Gmbh | Verfahren zur Beschichtung von metallischen Oberflächen mit einem Aktivierungsmittel vor dem Phosphatieren |
WO2010066765A1 (de) | 2008-12-09 | 2010-06-17 | Chemetall Gmbh | Verfahren zur beschichtung von metallischen oberflächen mit einem aktivierungsmittel vor dem phosphatieren |
DE102018216216A1 (de) * | 2018-09-24 | 2020-03-26 | Thyssenkrupp Ag | Verfahren zur Verbesserung der Phosphatierbarkeit von metallischen Oberflächen, welche mit einer temporären Vor- bzw. Nachbehandlung versehen werden |
DE102019134298A1 (de) * | 2019-12-13 | 2021-06-17 | Thyssenkrupp Steel Europe Ag | Verfahren zum Herstellen eines Stahlflachprodukts mit einer metallischen Schutzschicht auf Basis von Zink und einer auf einer Oberfläche der metallischen Schutzschicht erzeugten Phosphatierschicht und derartiges Stahlflachprodukt |
WO2021116318A1 (de) | 2019-12-13 | 2021-06-17 | Thyssenkrupp Steel Europe Ag | Verfahren zum herstellen eines stahlflachprodukts mit einer metallischen schutzschicht auf basis von zink und einer auf einer oberfläche der metallischen schutzschicht erzeugten phosphatierschicht und derartiges stahlflachprodukt |
Also Published As
Publication number | Publication date |
---|---|
JPH04254589A (ja) | 1992-09-09 |
JP3063921B2 (ja) | 2000-07-12 |
CA2040859A1 (en) | 1991-10-22 |
CA2040872A1 (en) | 1991-10-22 |
ZA912943B (en) | 1992-12-30 |
BR9101616A (pt) | 1991-12-10 |
DE59101978D1 (de) | 1994-07-28 |
DE4012795A1 (de) | 1991-10-24 |
ATE107711T1 (de) | 1994-07-15 |
EP0454211A1 (de) | 1991-10-30 |
ES2055518T3 (es) | 1994-08-16 |
US5160551A (en) | 1992-11-03 |
CA2040859C (en) | 2000-11-21 |
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