EP1646459B2 - Procede de production d'un composant trempe sous pression - Google Patents

Procede de production d'un composant trempe sous pression Download PDF

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Publication number
EP1646459B2
EP1646459B2 EP04741163.2A EP04741163A EP1646459B2 EP 1646459 B2 EP1646459 B2 EP 1646459B2 EP 04741163 A EP04741163 A EP 04741163A EP 1646459 B2 EP1646459 B2 EP 1646459B2
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EP
European Patent Office
Prior art keywords
component
coating
component blank
press
blank
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 - Fee Related
Application number
EP04741163.2A
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German (de)
English (en)
Other versions
EP1646459A1 (fr
EP1646459B1 (fr
Inventor
Michael Bayer
Martin Brodt
Leonid Levinski
Victor Samoilov
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.)
THERMISSION AG
Original Assignee
Thermission AG
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Filing date
Publication date
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Publication of EP1646459B1 publication Critical patent/EP1646459B1/fr
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D35/00—Combined processes according to or processes combined with methods covered by groups B21D1/00 - B21D31/00
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C21D1/673—Quenching devices for die quenching
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/60—After-treatment
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • 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
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49616—Structural member making
    • Y10T29/49622—Vehicular structural member making
    • 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
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49826—Assembling or joining
    • Y10T29/49885—Assembling or joining with coating before or during assembling
    • 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
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49826—Assembling or joining
    • Y10T29/49888—Subsequently coating
    • 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
    • Y10T428/8305—Miscellaneous [e.g., treated surfaces, etc.]

Definitions

  • the invention relates to a method for producing a press-hardened component.
  • Such a material is e.g. the precoated boron steel marketed by Usinor under the trader Usibor 1500.
  • the steel is provided with an AlSi coating which, among other things, exhibits advantageous corrosion-inhibiting properties in the course of the subsequent heat treatment.
  • the component is subjected to a preforming cut or a trimming step before the actual hot forming.
  • a preforming cut or a trimming step before the actual hot forming.
  • This is for example in the DE 101 49 221 C1 described.
  • a method may cause corrosion problems because a commonly applied tape coating will be damaged during preforming.
  • the object of the invention is to specify a press-hardened component as well as a production method for press-hardened components, which enables reliable corrosion protection for precoated, hot-workable steels.
  • An embodiment of the process according to the invention for the production of press-hardened components comprises the following processing steps: from the precoated semi-finished product, a component blank is formed by a cold forming process, in particular a drawing process; the component blank is trimmed at the edge on a part of the wall to be produced approximately corresponding boundary contour; the trimmed component blank is heated and press-hardened in a hot-forming tool; the press-hardened component blank is coated with a corrosion-protecting layer in a coating step, wherein the second layer is applied to the press-hardened component blank by a thermal diffusion method, and wherein the second layer is deposited on both the pre-coating and uncoated areas of the component blank is deposited.
  • this embodiment of the invention makes it possible to design the component manufacturing process in such a way that it is possible to dispense with the procedurally complex and costly final trimming of the hardened component.
  • the edge regions are therefore already cut in the uncured state of the component and not only - as usual in hot forming usual - after the heating and hardening process.
  • By pruning the workpiece already in the soft state significantly lower cutting forces are required than for cold-cutting hardened materials, resulting in reduced tool wear and a reduction in the maintenance cost of the cutting tools.
  • the risk of rapid cracking due to the high notch sensitivity of these materials is significantly reduced when trimming the high strength material in the uncured state.
  • the pre-coating provided on the semifinished product avoids scaling of the trimmed component blank in the hardening process, and the requirements for an inert atmosphere during curing can be reduced. In addition, the pre-coating prevents decarburization of the material during curing.
  • a further layer which protects against corrosion is applied, so that the component is completely coated, ie also at the edges.
  • the layer is applied to the press-hardened component blank by a thermal diffusion method, a readily controllable method can be used, with which preferably a layer of zinc or a zinc alloy can be applied, which is also suitable for complex component geometries and edge layering is.
  • the layer thickness can be adjusted selectively between a few microns and over 100 microns. A thermal load of the component is low.
  • Components can be coated regardless of their size, dimensions, configuration, complexity and weight.
  • a cleaning before the coating step with a dry cleaning, in particular blasting of the press-hardened component blank with glass particles or zinc particles, can be omitted, since the precoating a scaling of the component blank during hot forming substantially omitted thereby a process step is saved; In addition, it is avoided that a small, but possibly disturbing component distortion is caused by a blasting of the components with particles.
  • a good adhesion between the two coatings results.
  • the second layer applied to the first layer of the precoat provides edge coating and coating of those areas where the first layer of the precoat e.g. was chipped in the pre-forming or cracked due to excessive friction.
  • the component blank is cleaned of residues after the coating step, for example with ultrasound, and passivated, a surface is formed which gives a good primer for coatings, in particular primers of paints or coatings themselves
  • the component blank is tempered after the coating step. It is particularly advantageous if the component blank is coated with a zinc-containing layer because an oxide is formed on the surface, which is suitable as a primer.
  • a press-hardened component in particular a body component, from a semifinished product of unhardened, hot-workable steel sheet, which has been produced according to at least one embodiment of the method according to the invention, is particularly suitable for mass production with a corresponding series production and combines a favorable weight reduction of the component with excellent corrosion protection.
  • FIGS. 1a to 1e schematically show an inventive method for producing a spatially shaped, press-hardened component 1 from a semifinished product 2.
  • a board 3 is used as a semifinished product 2, which is cut out of a developed coil 5.
  • a composite sheet are used, as for example in the DE 100 49 660 A1 is described and which consists of a base plate and at least one reinforcing plate.
  • a Taylored Blank can be used, which consists of several welded together sheets of different material thickness and / or different material properties.
  • the semifinished product 2 may be a three-dimensionally shaped sheet-metal part produced by any forming process which is to undergo further deformation and a strength and / or rigidity increase with the aid of the method according to the invention.
  • the semifinished product 2 consists of an unhardened, hot-forming steel sheet.
  • a particularly preferred material is a boron-containing tempering steel, e.g. Usibor 1500, Usibor 1500 P or Usibor 1500 PC, which are distributed by the company Usinor under these trade names.
  • the board 3 ( Fig. 1a ) from a developed and straightened Section of a coil 5 cut out of a precoated, hot-forming sheet.
  • the coating is a coating of aluminum or an aluminum alloy, in particular a silicon-containing aluminum alloy AlSi.
  • the thermoformable material is at this time in an uncured state, so that board 3 can be easily cut using conventional mechanical cutting means 4, for example a scissors.
  • the cutting of the board 3 is advantageously carried out with the help of a platinum press 6, which ensures an automated feed of the coil 5 and an automatic punching and removal of the cut-out board 3.
  • the cut out in this way board 3 is in 2a shown in a schematic perspective view.
  • the cut-out blanks 3 are deposited on a stack 7 and fed in stacked form to a cold-forming station 8 (FIG. Fig. 1b ).
  • a component blank 10 is formed in a second process step II from the circuit board 3 by means of the cold forming tool 8, for example a two-stage deep drawing tool 9.
  • the board 3 has edge regions 11 which protrude beyond an outer contour 12 of the component 1 to be molded.
  • the component blank 10 is formed close to the final contour.
  • near-net shape should be understood to mean that those parts of the geometry of the finished component 1 which are associated with a macroscopic flow of material are completely formed in the component blank 10 after the cold-forming process has been completed. After completion of the cold forming process, only slight conformations of shape are required to produce the three-dimensional shape of the component 1, which require a minimum (local) material flow; the component blank 10 is in Fig. 2b shown.
  • the near-net shape shaping can take place in a single deep-drawing step, or it can take place in several stages ( Fig. 1b ).
  • the component blank 10 is inserted into a cutting device 15 and cut there (process step III, Hg. 1c).
  • the material is still in the uncured state at this time, so trimming can be accomplished by conventional mechanical cutting means 14 such as cutting knives, folding and / or punching tools.
  • a separate cutting device 15 may be provided.
  • the cutting means 14 may be integrated into the last stage 9 'of the deep-drawing tool 9, so that in the last deep-drawing stage 9' in addition to the final shaping of the sheet metal blank 10, the edge trimming takes place.
  • the process steps II and III are integrated in a single processing station, in which the forming and cutting is carried out fully automatically.
  • the removal of the component blank 17 from the processing station can be automated or there may be a manual removal and stacking of the component blanks 17.
  • the trimmed component blank 17 is subjected to hot working in a hot forming area 26, in the course of which it is formed and hardened to a final shape of the component 1.
  • the trimmed component blank 17 is inserted by a manipulator 20 in a continuous furnace 21, where it is heated to a temperature which is above the structural transformation temperature in the austenitic state; Depending on the grade of steel, this corresponds to heating to a temperature between 700 ° C and 1100 ° C.
  • a favorable range is between 900 ° C and 1000 ° C.
  • the atmosphere of the continuous furnace can be rendered inert by the addition of a protective gas, but the precoating of the blanks 3 already prevents at least a full-surface scaling of the blank surface.
  • the uncoated interfaces of the edge contour 12 'of the trimmed component blanks 17 represent only a very small area ratio of the component blank 17, so that adhesion of a layer applied later is virtually unaffected.
  • a suitable inert gas for inertization is e.g. Carbon dioxide or nitrogen.
  • the heated trimmed component blank 17 is then inserted by means of a manipulator 22 in a hot-forming tool 23, in which the three-dimensional shape and the edge contour 12 'of the trimmed component blank 17 are brought to their desired level. Since the trimmed component blank 17 already has near net shape dimensions, only a slight adaptation of the shape is necessary during hot forming.
  • the hot forming tool 23 the trimmed component blank 17 is finished and rapidly cooled, whereby a fine-grained martensitic or bainitic Weikstoffge Stahlge isIchelit. This step corresponds to a hardening of the component blank 18 and allows a targeted adjustment of the material strength. Details of such a curing process are eg in the DE 100 49 660 A1 described.
  • the hardened component blank 18 is taken out of the hot forming tool 23 with a manipulator and optionally stacked until further processing. Because of the near-contour near the Warnumform process trimming the component blank 10 and the shape adjustment of the edge contour 12 'in hot forming tool 23, the component 18 after completion of the hot forming process already the desired outer contour 24 of the finished component 1, so that after the hot forming no time-consuming trimming the edge of the component is necessary.
  • the component blank 18 can be quenched in a cooled hot forming tool 23. Since the surface is not scaled by the layer 33 of the precoating, a subsequent cleaning can be omitted.
  • the cycle times in the production method are advantageously short.
  • the cooling of the component blank 18 is a possible bottleneck.
  • air-hardening or water-hardening materials for the components 1 can be used.
  • the component blank 18 then only needs to cool down until a sufficient heat resistance, rigidity and associated dimensional accuracy of the component blank 18 is reached. Then, the component blank 18 can be removed from the tool 23, so that the further heat treatment process takes place in the air or in water outside of the tool 23, which then very quickly after a few seconds again for receiving further component blanks 17 is available
  • the press-hardened component blank 18 is coated in a coating process with a corrosion of the component 1 preventing layer 34.
  • drums 31 are charged with the press-hardened component blanks 18 and a zinc-containing powder, preferably a zinc alloy or a zinc-containing mixture, closed and introduced into a coating installation 30.
  • the component blanks 18 are heated slowly at about 5-10 K / min with slow rotation of the drums 31 to about 300 ° C.
  • the zinc or zinc alloy is distributed substantially homogeneously over the entire surface of the component blanks 18 and bonds to the surface.
  • a uniform layer thickness arises on the component blanks 18, which can be set arbitrarily between a few ⁇ m and more than 100 ⁇ m, preferably between 5 ⁇ m and 120 ⁇ m.
  • the layer 34 is weldable and gives a tensile strength that can be more than 1300 MPa for a component 1 made of BTR 165. In the thermal diffusion process virtually no residues or emissions to the environment.
  • the coating process is completed with a passivation process in an adjacent passivation station 35, in which the drums 31 are discharged from the coating system 30, cooled in a cooling station 36, ultrasonically freed of residues of the coating powder in a cleaning station 37 and in a tempering station 38 at a temperature of about 200 ° C for about 1 h, wherein the layer 34 is passivated.
  • suitable passivating additives may also be added. Then the finished corrosion-protected components 1 can be removed from the drum 31.
  • the press-hardened, coated component 1 is particularly suitable as a body component in vehicle construction, which are produced in large quantities.
  • the method according to the invention enables advantageous process control with short cycle times, all process steps have industrialization potential.
  • a precoated material it is possible to use conventional pre-forming.
  • a conventional forming and trimming is possible even with high-strength materials, so that - when using the manufacturing process according to FIG. 1 -
  • the costly laser cutting can be replaced at high volumes costly.
  • Sheet metal components can be protected by this manufacturing method already in the development by conventional forming simulation on their production.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
  • Coating With Molten Metal (AREA)
  • Heat Treatment Of Articles (AREA)

Claims (3)

  1. Procédé de production de composants, en particulier de carrosserie, trempés sous pression à partir d'un produit semi-fini (2) constitué d'une tôle d'acier non trempée pouvant être formée à chaud, dans lequel les étapes suivantes sont exécutées:
    - une ébauche de composant (10) est formée par un procédé de formage à froid, en particulier un procédé d'emboutissage, à partir du produit semi-fini (2) prérevêtu d'une première couche (33);
    - les bords de ladite ébauche de composant (10) sont découpés de façon à obtenir un contour (12') correspondant sensiblement à celui du composant à produire (1);
    - l'ébauche de composant découpée (17) est chauffée et trempée sous pression dans un outil de formage à chaud (23);
    - l'ébauche de composant trempée sous pression (18) est recouverte d'une seconde couche (34) anticorrosion lors d'une étape de revêtement, dans lequel ladite seconde couche (34) est appliquée sur ladite ébauche de composant (18, 18') trempée sous pression par un procédé de diffusion thermique et dans lequel la seconde couche (34) est déposée non seulement sur le prérevêtement (33) mais encore sur des parties non-revêtues de ladite ébauche de composant (18, 18').
  2. Procédé selon la revendication 1, caractérisé en ce que ladite ébauche de composant (18, 18') revêtue est nettoyée de résidus de ladite étape de revêtement.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que ladite ébauche de composant (18, 18') revêtue est malléabilisée après l'étape de revêtement.
EP04741163.2A 2003-07-22 2004-07-20 Procede de production d'un composant trempe sous pression Expired - Fee Related EP1646459B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2003133166 DE10333166A1 (de) 2003-07-22 2003-07-22 Pressgehärtetes Bauteil und Verfahren zur Herstellung eines pressgehärteten Bauteils
PCT/EP2004/008087 WO2005009642A1 (fr) 2003-07-22 2004-07-20 Composant trempe sous pression et procede de production d'un composant trempe sous pression

Publications (3)

Publication Number Publication Date
EP1646459A1 EP1646459A1 (fr) 2006-04-19
EP1646459B1 EP1646459B1 (fr) 2010-05-05
EP1646459B2 true EP1646459B2 (fr) 2019-01-02

Family

ID=34042013

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04741163.2A Expired - Fee Related EP1646459B2 (fr) 2003-07-22 2004-07-20 Procede de production d'un composant trempe sous pression

Country Status (6)

Country Link
US (1) US8127449B2 (fr)
EP (1) EP1646459B2 (fr)
JP (1) JP2006529002A (fr)
DE (2) DE10333166A1 (fr)
WO (1) WO2005009642A1 (fr)
ZA (1) ZA200600594B (fr)

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US8307680B2 (en) 2006-10-30 2012-11-13 Arcelormittal France Coated steel strips, methods of making the same, methods of using the same, stamping blanks prepared from the same, stamped products prepared from the same, and articles of manufacture which contain such a stamped product
EP2014777B1 (fr) * 2007-07-11 2013-01-09 Neue Materialien Bayreuth GmbH Procédé et dispositif pour le traitement thermique d'une tôle métallique
EP2045360B1 (fr) * 2007-10-02 2011-11-30 ThyssenKrupp Steel Europe AG Procédé de fabrication d'un composant en acier par façonnage à chaud et composant en acier fabriqué par façonnage à chaud
DE102007057855B3 (de) 2007-11-29 2008-10-30 Benteler Automobiltechnik Gmbh Verfahren zur Herstellung eines Formbauteils mit mindestens zwei Gefügebereichen unterschiedlicher Duktilität
JP5155646B2 (ja) * 2007-12-13 2013-03-06 アイシン高丘株式会社 熱間プレス成形装置及び熱間プレス成形方法
EP2287343B1 (fr) * 2008-08-28 2012-12-26 Hyundai Steel Company Procédé et appareil de durcissement par pressage continu
JP5288385B2 (ja) * 2008-08-28 2013-09-11 ヒュンダイ スチール カンパニー プレス硬化工程用加熱炉装置
DE102008043401B4 (de) * 2008-11-03 2017-09-21 Volkswagen Ag Verfahren und Vorrichtung zur Herstellung von Blechbauteilen mittels Warmumformung sowie dadurch hergestellte Blechbauteile
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JP5431251B2 (ja) * 2010-06-10 2014-03-05 株式会社神戸製鋼所 曲げ加工用金型、これを用いた自動車用サスペンションアームの製造装置およびその製造方法
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EP1646459A1 (fr) 2006-04-19
US8127449B2 (en) 2012-03-06
DE502004011133D1 (de) 2010-06-17
EP1646459B1 (fr) 2010-05-05
US20070175040A1 (en) 2007-08-02
JP2006529002A (ja) 2006-12-28
WO2005009642A1 (fr) 2005-02-03
DE10333166A1 (de) 2005-02-10

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