EP1646735B1 - Verfahren zur behandlung der oberflächen von blechen und bändern aus aluminiumlegierung - Google Patents

Verfahren zur behandlung der oberflächen von blechen und bändern aus aluminiumlegierung Download PDF

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Publication number
EP1646735B1
EP1646735B1 EP04767292A EP04767292A EP1646735B1 EP 1646735 B1 EP1646735 B1 EP 1646735B1 EP 04767292 A EP04767292 A EP 04767292A EP 04767292 A EP04767292 A EP 04767292A EP 1646735 B1 EP1646735 B1 EP 1646735B1
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EP
European Patent Office
Prior art keywords
treatment
process according
bath
strip
sheet
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Expired - Lifetime
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EP04767292A
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English (en)
French (fr)
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EP1646735A2 (de
Inventor
Mohamed Benmalek
Evelyne Hank
Ravi Shahani
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Constellium Issoire SAS
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Alcan Rhenalu SAS
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y10T428/12743—Next to refractory [Group IVB, VB, or VIB] metal-base component

Definitions

  • the invention relates to the field of surface treatments of aluminum alloy sheets and strips, as well as parts stamped from these sheets, more particularly to type 6xxx or 5xxx alloys according to the designation of the Aluminum Association, intended for in particular to the manufacture of motor vehicle body parts.
  • Aluminum is increasingly used in the automotive industry to reduce the weight of vehicles and thus fuel consumption and the discharge of pollutants and greenhouse gases.
  • the sheets are used in particular for the manufacture of body skin parts, in particular the openings.
  • This type of application requires a set of properties, sometimes antagonistic, in terms of mechanical strength, corrosion resistance, formability; with an acceptable cost for mass production.
  • chromium-based chemical conversions are used. Although still often used, these conversions may disappear for environmental reasons for fear of the presence of hexavalent chromium.
  • a surface preparation suitable for assembly operations may be necessary. Performing these pre-treatments is time consuming and expensive. Indeed the formation of the surface layer requires a series of manipulations of different baths with a number of tanks that may be greater than 8.
  • a standard treatment line consists of 2 alkaline degreasing baths, followed by 2 baths of rinsing, an acid neutralization bath, a specific treatment bath, followed by 2 rinsing baths and a drying step. Most of these baths are sometimes heated up to 60 ° C, which is energy intensive.
  • the invention therefore proposes to carry out a pre-treatment on aluminum alloy strips or sheets adapted to the requirements of the automobile industry, while minimizing the handling operations of the strip or sheet.
  • it aims to provide ready-to-assemble sheets for car body parts, with high performance for the adhesion of adhesives and adhesives used in automotive and spot welding, as well as a stability in the time of the quality of surface.
  • the invention relates to a method for surface treatment of a strip, a sheet or a part stamped from an aluminum alloy sheet or strip, consisting of a surface preparation using an atmospheric plasma, and a chemical conversion treatment using at least one of Si, Ti, Zr, Ce, Co, Mn, Mo or V to form the conversion layer.
  • the conversion treatment can be carried out using a bath containing between 1 and 10% by weight of at least one salt of at least one of the elements Si, Ti, Zr, Ce, Co, Mn, Mo or V, and in this case the process preferably comprises, at the end of the treatment, a spin with a roller. It can be carried out by immersion in the bath, by spraying the bath on the strip, the sheet or the workpiece, or by coating the bath with a roller, according to a "no rinse" technique.
  • the conversion treatment can also be done using an atmospheric plasma in which the plasmagenic gas comprises a compound of at least one of the elements Si, Al, Ti, Zr, Ce, Co, Mn, Mo or V
  • the element of the compound added to the plasma gas is preferably silicon.
  • the invention is based on the finding made by the applicant that, when the chemical conversion treatment is preceded by a preparation, for example a degreasing, using an atmospheric plasma, this treatment can be considerably simplified compared with to the treatments of the prior art made for the same purpose, and that one could be satisfied with a fast treatment, for example of the "no-rinse" type using a conversion bath with spinning with a roller, but also a conversion treatment performed, too, using an atmospheric plasma.
  • Atmospheric plasma techniques have developed significantly in recent years and many applications have been proposed, especially in the treatment of metals.
  • the patent application WO 02/39791 discloses a method and apparatus for atmospheric plasma treatment of a conductive surface, and in one of the examples mentions the cleaning of an aluminum foil from the rolling grease residues.
  • a treatment of this type has, surprisingly, proved more favorable than the usual chemical degreasing treatments for the implementation of the subsequent chemical conversion, the plasma performing both the degreasing and the modification of the natural oxide. present on the surface of aluminum.
  • the atmospheric plasma can also be used for the formation of the conversion layer itself, provided that the compound containing the decomposition of the desired element for the conversion layer is added to the plasma-forming gas.
  • the chemical conversion treatment is preferably carried out using a solution containing metal elements such as Si, Ti, Zr, Ce, Co, Mn, Mo, V or combinations of these elements, for example a Ti / Zr product, which can chemically react with the metal surface to form a more stable oxide layer than the natural oxide. It has been found that this operation can be carried out although the strip, the sheet or the piece remains in contact with the liquid only for a very short time. In the case of tapes, this allows on-line processing compatible with the production speeds of these tapes.
  • metal elements such as Si, Ti, Zr, Ce, Co, Mn, Mo, V or combinations of these elements
  • chromium-containing reagents it is preferable to exclude chromium-containing reagents to avoid the possible formation of products containing hexavalent chromium.
  • the additives in the treatment baths are at a very low concentration, less than 10%, and preferably between 1 and 5%.
  • the aggressiveness of the bath in terms of acidity is limited by using baths of pH between 3 and 11.
  • the oxide formed combines both the aluminum and the element present in the bath.
  • Many bath compositions are available on the market, such as containing salts of titanium, zirconium, cerium, cobalt, manganese, vanadium or silicon compounds.
  • the strip, the sheet or the workpiece is preferably dewatered using a roller according to the so-called “no-rinse” technique known to those skilled in the art, this technique being particularly suitable for continuous treatment of tapes.
  • the layers formed can be controlled by weight gain, X-ray fluorescence or ESCA analysis, the latter two techniques giving information on the constituents of the layer and, in addition, for ESCA, on the chemical bonds in which the elements are involved. .
  • the oxide thickness is very small, in the range 5 to 50 nm.
  • ESCA analysis can give an estimate of the oxide layer if its thickness is less than about 6 nm and if the surface contamination is low. Indeed, most often, the surface is covered with a layer of carbon contamination that disturbs the measurement.
  • transmission electron microscopy can be used after sample preparation by microtomy. This technique makes it possible to calibrate the measurements made by ESCA.
  • this resistance is less than 20 or 15 ⁇ , which is compatible with the requirements of the automotive industry.
  • the conversion layer is obtained by a new passage in an atmospheric plasma, the plasmagenic gas, for example air, argon or a rare gas plus oxygen mixture.
  • the plasmagene gas is enriched with a compound which decomposes the metal element of the Si, Al, Ti, Zr, Ce, Co, Mn, Mo or V group which it is desired to include in the conversion layer.
  • One of the most efficient elements is silicon, which leads to an SiO x type conversion layer where x is close to 2.
  • Silicon can come for example from the decomposition of an organic compound containing silicon or silicon and oxygen, such as tetra-ethyl-disiloxane, tetra-methyl-disiloxane, hexa-methyl-disiloxane or hexamethyldisilazane, mixed with the argon used for the plasmagen mixture.
  • an organic compound containing silicon or silicon and oxygen such as tetra-ethyl-disiloxane, tetra-methyl-disiloxane, hexa-methyl-disiloxane or hexamethyldisilazane
  • the oxide layer obtained by this embodiment has a uniform thickness layer 10 to 30 nm on which is deposited a set of aggregates nanobeads more or less interconnected, with an excess thickness may exceed 200 nm.
  • this structure of the oxide layer comes from its formation in two successive stages. Firstly, the growth of a uniform and continuous barrier layer, where silicon combines with oxygen, and possibly other elements present on the surface, to form an amorphous deposit, then the growth of silica nanobeads forming aggregates, all the more important that the number of passages (equivalent to a longer transit time of the surface in front of the plasma) is higher. These aggregates contribute, by ensuring mechanical anchoring, to improve the adhesion of the base oxide layer in case of bonding.
  • the method according to the invention gives results as good as a conventional treatment comprising the passage in degreasing baths, pickling and rinsing, which leads to a shorter treatment time and reduced cost. This is even more pronounced when using a "no rinse” conversion or a plasma conversion, which avoids the passage into a rinsing bath. Finally, the use of compounds without chromium makes it possible to better respect the environment and to simplify the treatment of the effluents.
  • the plasma treatment is performed with several passes in front of the torch to accumulate energy on the metal avoiding excessive heating that could lead to an early fusion.
  • the ESCA analysis shows a clear decrease of the carbon layer, which goes from 40-50% of surface carbon to 25-30%. This value may still appear high, but it is probably related to the fact that samples are analyzed after exposure to the air.
  • the oxide layer passes from its side by a value of between 3 and 5 nm to a value of between 6 and 8 nm depending on the alloy.
  • the ESCA analysis also indicates a magnesium enrichment of the surface oxide, magnesium oxide accounting for nearly one-third of the surface oxide, but paradoxically this magnesium level does not seem to hinder adhesion, contrary to this which is generally accepted.
  • the figure 1 shows the crack propagation for the conversion layers made according to the invention with a bath containing the products A and C, as well as for reference samples degreased with solvent Viapred from SID (product D). It is found that the samples treated according to the invention have, whatever the alloy used, a better behavior than the reference treatment, and are therefore suitable for bonding.
  • Samples of aluminum alloy sheets AA5182 in the 0 (annealed) state of thickness 1 mm, and of AA6016 alloy in the T4 state with a thickness of 1.2 mm were prepared.
  • the samples were degreased by atmospheric plasma treatment using a device such as that described in the patent application. WO 02/39791 and using as reactive gas hexamethyldisilazane.
  • the ESCA analysis whose results are shown in Table 2, clearly shows the presence of this layer of silicon oxide. Its thickness depends on the treatment conditions. Thicknesses of 100 to 300 nm could thus be deposited by the atmospheric plasma technique. This layer masks the other elements present at the extreme surface of the metal, but for the small thicknesses one can still detect elements such as A1 or Mg.
  • the table gives the atomic percentages of the elements on the surface of the samples.
  • Sample 5182-H22 SiO2 # 3 shows different values from the other samples.
  • the carbon content is important while it shows practically no silica on the surface.
  • This sample was analyzed on the untreated side, which confirms the effect of stripping and treatment. Other changes in carbon content can be attributed to contamination when handling treated plates. However, the detection of Al and Mg elements in a substantially larger amount may indicate that the thickness is slightly lower.
  • the figure 2 shows the crack propagation for atmospheric plasma deposition carried out on alloys 6016 and 5182 and used with or without lubricant, as well as for reference samples converted chemically according to methods used by some car manufacturers. It is found that the treated samples have, whatever the alloy used, a better behavior than the reference treatments. Bonding in the absence of lubricant, which is performed immediately after treatment, gives a slightly better result. Likewise, the 5182 alloy in the O state behaves slightly better than in the H22 state. The bonding operations for the lubricant-coated plates were carried out after storage in the lubricated state for a period of more than 1 1 ⁇ 2 months in a normal laboratory atmosphere. This shows the robustness of the atmospheric plasma treatment which considerably improves the surface properties of the metal.
  • Table 3 shows the failure mode of the joints bonded during the cleavage test. Table 3 Cases tested ⁇ 96-0 origin 5 h 48 h 96 h End 6016 SiO2 # 1 No lube 3.3 RC RC RC RC RC 6016 SiO2 # 1 DC3 2.7 RC RC RC RC 6016 SiO2 # 2 DC3 4.1 RC RC RC RC 6016 SiO2 # 3 DC3 4.5 RC RC RC RC 5182 O SiO2 # 1 No lube 2.7 RC RC RC RC 5182 O SiO2 # 1 6130 2.9 RC RC80 RC80 RC80 RC 5182 O SiO2 # 2 6130 3.6 RC RC90 RC85 RC85 RC 5182 O SiO2 # 3 6130 3.7 RC RC RC RC 5182 H22 SiO2 # 1 6130 * 4.3 RC RC RC RC RC 5182 H22 SiO2 # 2

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Chemical Vapour Deposition (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Finishing Walls (AREA)
  • Arc Welding In General (AREA)
  • Chemically Coating (AREA)
  • Cleaning In General (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Coating With Molten Metal (AREA)

Claims (12)

  1. Verfahren zur Oberflächenbehandlung eines Bandes, eines Blechs oder eines aus einem Blech oder Band aus Aluminiumlegierung tiefgezogenen Teils, bestehend aus einer Oberflächenvorbereitung mit einem Atmosphärenplasma und einem chemischen Umwandlungsverfahren unter Verwendung wenigstens eines der Elemente Si, Ti, Zr, Ce, Co, Mn, Mo oder V zur Ausbildung der Umwandlungsschicht auf dem Band, dem Blech oder dem Teil.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Aluminiumlegierung eine Legierung der Serie 5000 oder der Serie 6000 ist.
  3. Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass die Umwandlungsbehandlung mit wenigstens einem Salz wenigstens eines der Elemente erfolgt.
  4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass die Umwandlungsbehandlung im Tauchbad erfolgt.
  5. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass die Umwandlungsbehandlung durch Aufsprühen der Badflüssigkeit auf das Band, das Blech oder das Teil erfolgt.
  6. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass die Umwandlungsbehandlung durch Walzenauftrag der Badflüssigkeit auf das Band, das Blech oder das Teil erfolgt.
  7. Verfahren nach einem der Ansprüche 3 bis 6, dadurch gekennzeichnet, dass das Behandlungsbad einen pH-Wert zwischen 3 und 11 hat.
  8. Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass die Umwandlungsbehandlung mit einem Atmosphärenplasma unter Verwendung eines Plasmagases erfolgt, welches eine Verbindung wenigstens eines der Elemente Si, Al, Ti, Zr, Ce, Co, Mn, Mo oder V enthält.
  9. Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, dass die Behandlungsgeschwindigkeit 5 m/min bis 600 m/min beträgt.
  10. Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, dass die Umwandlungsschicht eine Dicke zwischen 5 und 300 nm hat.
  11. Verwendung von Blechen oder Bändern, hergestellt durch das Verfahren nach einem der Ansprüche 1 bis 10, für die Herstellung geklebter oder punktgeschweißter Teile.
  12. Verwendung von Blechen oder Bändern, hergestellt durch das Verfahren nach einem der Ansprüche 1 bis 10, für die Herstellung von Kraftfahrzeugkarosserieteilen.
EP04767292A 2003-06-11 2004-06-09 Verfahren zur behandlung der oberflächen von blechen und bändern aus aluminiumlegierung Expired - Lifetime EP1646735B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0307004A FR2856079B1 (fr) 2003-06-11 2003-06-11 Procede de traitement de surface pour toles et bandes en alliage d'aluminium
PCT/FR2004/001426 WO2004111300A2 (fr) 2003-06-11 2004-06-09 Procede de traitement de surface pour toles et bandes en alliage d’aluminium

Publications (2)

Publication Number Publication Date
EP1646735A2 EP1646735A2 (de) 2006-04-19
EP1646735B1 true EP1646735B1 (de) 2008-11-12

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Country Status (13)

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US (1) US20070026254A1 (de)
EP (1) EP1646735B1 (de)
JP (1) JP5183062B2 (de)
KR (1) KR101102142B1 (de)
AT (1) ATE414187T1 (de)
AU (1) AU2004247920A1 (de)
BR (1) BRPI0411326A (de)
CA (1) CA2528702A1 (de)
DE (1) DE602004017737D1 (de)
ES (1) ES2318327T3 (de)
FR (1) FR2856079B1 (de)
NO (1) NO20055805L (de)
WO (1) WO2004111300A2 (de)

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JP2003049272A (ja) * 2001-08-07 2003-02-21 Konica Corp 大気圧プラズマ処理装置、大気圧プラズマ処理方法及び大気圧プラズマ処理装置用の電極システム
JP2003129246A (ja) * 2001-10-26 2003-05-08 Sekisui Chem Co Ltd 放電プラズマ処理装置
FR2850643A1 (fr) * 2003-01-30 2004-08-06 Neopost Ind Dispositif de reception d'enveloppes

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10125424B2 (en) 2012-08-29 2018-11-13 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates
US10920324B2 (en) 2012-08-29 2021-02-16 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates

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JP5183062B2 (ja) 2013-04-17
WO2004111300A2 (fr) 2004-12-23
KR20060027328A (ko) 2006-03-27
US20070026254A1 (en) 2007-02-01
CA2528702A1 (fr) 2004-12-23
DE602004017737D1 (de) 2008-12-24
FR2856079A1 (fr) 2004-12-17
NO20055805L (no) 2006-03-10
KR101102142B1 (ko) 2012-01-02
FR2856079B1 (fr) 2006-07-14
WO2004111300A3 (fr) 2005-02-17
AU2004247920A1 (en) 2004-12-23
JP2006527306A (ja) 2006-11-30
ATE414187T1 (de) 2008-11-15
EP1646735A2 (de) 2006-04-19
ES2318327T3 (es) 2009-05-01
NO20055805D0 (no) 2005-12-07
BRPI0411326A (pt) 2006-07-25

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