EP0613964B1 - Procédé facilitant la déformation à froid - Google Patents
Procédé facilitant la déformation à froid Download PDFInfo
- Publication number
- EP0613964B1 EP0613964B1 EP94200388A EP94200388A EP0613964B1 EP 0613964 B1 EP0613964 B1 EP 0613964B1 EP 94200388 A EP94200388 A EP 94200388A EP 94200388 A EP94200388 A EP 94200388A EP 0613964 B1 EP0613964 B1 EP 0613964B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- calculated
- phosphating solution
- phosphate
- dipped
- ferrous materials
- 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
- C23C22/34—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
-
- 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
-
- 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
- C23C22/362—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 also zinc cations
Definitions
- the invention relates to a method for facilitating the non-cutting cold forming of ferrous materials by applying a phosphate coating in an immersion process by means of an aqueous acid phosphating solution which contains zinc, Mg and phosphate ions as well as oxidizing agents and is practically free of Fe-II ions.
- Phosphate coatings are usually applied to metal surfaces in order to improve their corrosion resistance and to increase the adhesion of the paint that is subsequently applied. Phosphate coatings also serve to facilitate non-cutting cold forming, whereby they themselves act as a "lubricant" by helping to avoid seizing or welding of material and tools or by binding a subsequently applied lubricant so that it is practically not removed during the forming process. In particular, the latter ability is of particular importance because only the combination of phosphate coating and lubricant enables multiple or strong cold forming, possibly without a new intermediate treatment with lubricant.
- Layer-forming here means the formation of phosphate coatings by means of phosphating solutions which, in addition to the phosphate ions, also predominantly Supply cations for coating formation.
- the cations of the phosphate coating usually originate from the treated metal itself, ie the phosphating solution essentially only provides the phosphate ions.
- EP-A-45110 describes a process for the production of phosphate coatings on iron or steel surfaces by immersion or flooding, in which phosphating solutions are used which contain at least 0.3% by weight of Zn and at least 0.3% by weight. % PO4 and contain at least 0.75 wt .-% NO3 or an equivalent, iron II non-oxidizing accelerator.
- the Zn: PO4 weight ratio should be greater than 0.8 and the iron (II) content to be set should be 0.05 to 1% by weight.
- the solutions described here can contain calcium, which can be partially or completely replaced by magnesium, and are suitable for the production of phosphate coatings, among other things. as preparation for cold forming.
- EP-A-403 241 it is known to form zinc phosphate coatings on metal surfaces with the aid of aqueous zinc phosphate solutions which contain 2 to 20 g / l zinc, 5 to 40 g / l phosphate and silicotungstic acid or silicotungstate in a concentration of 0.005 to 20 g / l (calculated as W) included.
- the phosphating solutions can contain nitrite, nitrobenzenesulfate, hydrogen peroxide, nitrate and chlorate as accelerators.
- nickel, cobalt, calcium and manganese in the phosphating solution that of magnesium is also mentioned in an amount of 0.5 to 10 g / l.
- the process has been described as being suitable for preparing metals for the subsequent cold forming.
- solutions which contain 0.4 to 30 g / l zinc, 4 to 30 g / l P2O5, 5 to 50 g / l NO3, and a maximum of 10 g / l Fe II and a maximum of 0.3 g / l Fe III.
- These solutions which May also contain up to 10 g / l of magnesium, are supplemented in a certain way and operated with a certain addition of oxidizing agent, so that the actual aim of this process - to be able to work essentially without waste water - can be achieved.
- the increased alkali resistance of the coatings containing mixed phosphates, which makes them particularly suitable as a primer for paints, is mentioned as an advantage for the magnesium content or for the calcium content of the phosphating solutions, which is shown to be equivalent.
- the object of the invention is to provide a method for facilitating the cold forming of ferrous materials by applying a phosphate coating, which avoids the disadvantages of the known methods, in particular does not pose any waste water problems, leads to firmly adhering coatings with a sufficient thickness for the cold forming and yet allows simple process control.
- the object is achieved by equipping the method of the type mentioned at the outset in accordance with the invention in such a way that the iron materials are immersed in a phosphating solution which is free of elements of the sixth subgroup of the Periodic Table of the Elements and free of nitrogen compounds, and 5 to 20 g / l zinc 1 to 15 g / l magnesium 10 to 26 g / l phosphate (calculated as P2O5) 1 to 15 g / l fluoroborate (calculated as BF4) 1 to 7 g / l chlorate (calc. As ClO3) contains and in which the weight ratio of Zn: Mg: BF4 is set to a value in the range from 1: (0.15 to 1): (0.15 to 1).
- a preferred embodiment of the invention accordingly provides that the ferrous materials are immersed in a phosphating solution 6 to 17 g / l zinc 2 to 5 g / l magnesium 13 to 20 g / l phosphate (calculated as P2O5) 2 to 5 g / l fluoroborate (calculated as BF4) 2 to 4 g / l chlorate (calculated as ClO3) contains.
- This embodiment of the invention as the further preferred embodiment with setting a weight ratio of Zn: Mg: BF4 of 1: (0.23 to 0.46): (0.23 to 0.46) is associated with the advantage that the Chemical consumption is very low, on the other hand, a particularly good phosphate layer formation is achieved.
- a phosphating solution which contains 5 to 40 g / l, preferably 10 to 30 g / l, of sulfate.
- chlorides and acetate additives are also possible to adjust the electroneutrality in the phosphating solution.
- they are less advantageous for reasons of a certain susceptibility to corrosion of the treated workpieces (chloride) or the comparatively high cost (acetate).
- the addition of sulfate also has the advantage that it has a favorable influence on the crystal structure of the phosphate layer produced, in that the absorption capacity and the anchoring of the lubricant normally applied are improved.
- the S value of the phosphating solution to be used should be in the range from 0.1 to 0.4.
- the S-value is the ratio of "free acid” - calculated as P2O5 - and the so-called “total acid Fischer", ie the total amount of P2O5, expressed as consumption of 0.1 n NaOH in ml for the titration of a 10 ml bath sample (cf. W. Rausch "The phosphating of metals", 2nd Ed., Eugen G. Leuze Verlag Saalgau 1988, pp. 299-304).
- Another advantageous embodiment of the invention provides that the ferrous materials are immersed in a phosphating solution which is nickel-free.
- the freedom from nickel has the advantage that the treatment of the rinse water or else the processed phosphating bath is easier before draining into the sewer and less problematic sludge is obtained as a result of the treatment. From the point of view of workplace hygiene, it is an advantage both in the phosphating plant and in the cold forming equipment (dust formation).
- the application temperature of the phosphating solution is unlimited within wide limits.
- the iron materials are immersed in a phosphating solution set at a temperature of 50 to 70 ° C. These are the optimal conditions with regard to layer formation speed and heat economy. At the aforementioned temperatures, the treatment time is generally between 3 and 15 minutes.
- the phosphating solution can be formulated as such from the individual components, but particularly expediently from a concentrate. In both cases, the cations are introduced, for example, as metal, oxide, carbonate, sulfate, phosphate, and possibly also as chlorate.
- the component can be added via alkali phosphate and / or phosphoric acid.
- the phosphating solutions used in the process according to the invention can contain, in addition to the components already mentioned, other additives known per se, but mostly in minor amounts. These include, for example, copper, manganese, calcium and sludge conditioning agents.
- the phosphating solution is applied in dipping, which also means flooding.
- phosphate coatings with a layer weight of approximately 5 to 15 g / m 2. This enables the layer weight to be adapted to the severity of the intended cold forming, the size of the workpiece and the like. Finally, when choosing the layer weight, it must also be considered whether a lubricant is subsequently applied or not.
- the workpieces are pretreated before phosphating in the usual way, such as by cleaning, pickling, rinsing and, if necessary, activating.
- a lubricant customary for cold forming processes is usually applied as aftertreatment. This can be done immediately after coating or after an intermediate rinse. The lubricant can also be applied immediately before the forming, if necessary also between the forming steps. If the purpose of the formation of zinc soaps is with the application of lubricant, care must be taken to ensure that the phosphate coating is sufficiently moist for the reaction.
- Soaps, oils and other auxiliaries for cold forming or emulsions of fatty acids or soaps, in particular with 8 to 18 carbon atoms in the acid anion, can be applied as lubricants. Because of the reaction with the cation of the phosphate coating already mentioned above, sodium and / or potassium soaps, in particular stearates, are particularly advantageous.
- the steel grade ST35 pipes were pulled at a speed of 60 m / min, the steel grade ST52 at a speed of 30 m / min.
Claims (9)
- Procédé facilitant la déformation à froid sans enlèvement de copeaux de produits ferreux par application d'un revêtement de phosphate par le procédé d'immersion au moyen d'une solution aqueuse acide de phosphatation, qui contient des ions de zinc, des ions de Mg et des ions phosphates, de même que des agents d'oxydation et qui est pratiquement exempte d'ions Fe (II), caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui est exempte d'éléments du sixième sous-groupe du système périodique des éléments, de même qu'exempte de composés de l'azote et qui contient
5 à 20 g/l de zinc
1 à 15 g/l de magnésium
10 à 26 g/l de phosphate (calculé sous forme de P₂O₅)
1 à 15 g/l de fluoroborate (calculé sous forme de BF₄)
1 à 7 g/l de chlorate (calculé sous forme de ClO₃)
et dans laquelle le rapport massique de Zn : Mg : BF₄ est réglé à une valeur dans la gamme de 1 : (0,15 à 1) : (0,15 à 1). - Procédé selon la revendication 1, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui contient
6 à 17 g/l de zinc
2 à 5 g/l de magnésium
13 à 20 g/l de phosphate (calculé sous forme de P₂O₅)
2 à 5 g/l de fluoroborate (calculé sous forme de BF₄)
2 à 4 g/l de chlorate (calculé sous forme de ClO₃). - Procédé selon la revendication 1 ou 2, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation dans laquelle le rapport massique de Zn : Mg : BF₄ est réglé à une valeur dans la gamme de 1 : (0,23 à 0,46) : (0,23 à 0,46).
- Procédé selon la revendication 1, 2 ou 3, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui contient 5 à 40 g/l de sulfate (calculé sous forme de SO₄).
- Procédé selon la revendication 4, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui contient 10 à 30 g/l de sulfate (calculé sous forme de SO₄).
- Procédé selon une ou plusieurs des revendications 1 à 5, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui présente une valeur S dans la gamme de 0,1 à 0,4.
- Procédé selon une ou plusieurs des revendications 1 à 6, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation qui est exempte de nickel.
- Procédé selon une ou plusieurs des revendications 1 à 7, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation réglée à une température de 50 à 70 °C.
- Procédé selon une ou plusieurs des revendications 1 à 8, caractérisé en ce qu'on immerge les produits ferreux dans une solution de phosphatation pendant une durée de 3 à 15 minutes.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4306446A DE4306446A1 (de) | 1993-03-02 | 1993-03-02 | Verfahren zur Erleichterung der Kaltumformung |
DE4306446 | 1993-03-02 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0613964A1 EP0613964A1 (fr) | 1994-09-07 |
EP0613964B1 true EP0613964B1 (fr) | 1995-11-08 |
Family
ID=6481724
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94200388A Expired - Lifetime EP0613964B1 (fr) | 1993-03-02 | 1994-02-15 | Procédé facilitant la déformation à froid |
Country Status (10)
Country | Link |
---|---|
US (1) | US5415701A (fr) |
EP (1) | EP0613964B1 (fr) |
JP (1) | JPH06322550A (fr) |
KR (1) | KR100324862B1 (fr) |
CN (1) | CN1040779C (fr) |
AT (1) | ATE130052T1 (fr) |
DE (2) | DE4306446A1 (fr) |
ES (1) | ES2081224T3 (fr) |
TW (1) | TW270901B (fr) |
ZA (1) | ZA941457B (fr) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4630326B2 (ja) * | 1999-08-09 | 2011-02-09 | 新日本製鐵株式会社 | 加工性に優れたリン酸塩処理亜鉛系めっき鋼板の製造方法 |
ATE399218T1 (de) | 2002-07-10 | 2008-07-15 | Chemetall Gmbh | Verfahren zur beschichtung von metallischen oberflächen |
DE10320313B4 (de) * | 2003-05-06 | 2005-08-11 | Chemetall Gmbh | Verfahren zum Beschichten von metallischen Körpern mit einer Phosphatierungslösung, Phosphatierungslösung und die Verwendung des beschichteten Gegenstandes |
DE10323305B4 (de) * | 2003-05-23 | 2006-03-30 | Chemetall Gmbh | Verfahren zur Beschichtung von metallischen Oberflächen mit einer Wasserstoffperoxid enthaltenden Phosphatierungslösung, Phosphatierlösung und Verwendung der behandelten Gegenstände |
TWI457433B (zh) * | 2008-01-30 | 2014-10-21 | Chemetall Gmbh | 將金屬表面施以一磷酸鹽層然後施以一潤滑劑層的方法 |
TWI457432B (zh) * | 2008-01-30 | 2014-10-21 | Chemetall Gmbh | 將金屬表面施以一含蠟的潤滑劑組成物的方法 |
TWI457431B (zh) * | 2008-01-30 | 2014-10-21 | Chemetall Gmbh | 將金屬表面施以一種潤滑劑組成物的方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1796102A1 (de) * | 1968-08-31 | 1972-02-17 | Metallgesellschaft Ag | Verfahren zum Aufbringen eines Phosphatueberzuges auf Oberflaechen von Eisen und Stahl |
FR2389683A1 (en) * | 1977-05-03 | 1978-12-01 | Parker Ste Continentale | Phosphating soln. contg. boron fluoride - for phosphating ferrous and non-ferrous surfaces, e.g. steel, zinc and aluminium |
GB2080835B (en) * | 1980-07-25 | 1984-08-30 | Pyrene Chemical Services Ltd | Prevention of sludge in phosphating baths |
ES2036666T3 (es) * | 1987-08-19 | 1993-06-01 | Metallgesellschaft Ag | Procedimiento para fosfatar metales. |
JPH0696773B2 (ja) * | 1989-06-15 | 1994-11-30 | 日本ペイント株式会社 | 金属表面のリン酸亜鉛皮膜形成方法 |
DE3927613A1 (de) * | 1989-08-22 | 1991-02-28 | Metallgesellschaft Ag | Verfahren zur erzeugung von phosphatueberzuegen auf metalloberflaechen |
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 |
-
1993
- 1993-03-02 DE DE4306446A patent/DE4306446A1/de not_active Withdrawn
-
1994
- 1994-02-15 AT AT94200388T patent/ATE130052T1/de not_active IP Right Cessation
- 1994-02-15 ES ES94200388T patent/ES2081224T3/es not_active Expired - Lifetime
- 1994-02-15 DE DE59400038T patent/DE59400038D1/de not_active Expired - Lifetime
- 1994-02-15 EP EP94200388A patent/EP0613964B1/fr not_active Expired - Lifetime
- 1994-02-18 TW TW083101372A patent/TW270901B/zh active
- 1994-02-28 KR KR1019940003802A patent/KR100324862B1/ko not_active IP Right Cessation
- 1994-02-28 CN CN94102150A patent/CN1040779C/zh not_active Expired - Fee Related
- 1994-03-02 US US08/204,984 patent/US5415701A/en not_active Expired - Lifetime
- 1994-03-02 JP JP6056641A patent/JPH06322550A/ja not_active Ceased
- 1994-03-02 ZA ZA941457A patent/ZA941457B/xx unknown
Also Published As
Publication number | Publication date |
---|---|
EP0613964A1 (fr) | 1994-09-07 |
CN1040779C (zh) | 1998-11-18 |
ZA941457B (en) | 1995-09-04 |
DE4306446A1 (de) | 1994-09-08 |
US5415701A (en) | 1995-05-16 |
JPH06322550A (ja) | 1994-11-22 |
KR940021761A (ko) | 1994-10-19 |
ES2081224T3 (es) | 1996-02-16 |
ATE130052T1 (de) | 1995-11-15 |
TW270901B (fr) | 1996-02-21 |
CN1093416A (zh) | 1994-10-12 |
DE59400038D1 (de) | 1995-12-14 |
KR100324862B1 (ko) | 2002-06-20 |
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