EP0820529B1 - Procede de fabrication de produits allonges finis a chaud, notamment du type barre ou tube, en acier fortement allie ou hypereutectoide - Google Patents

Procede de fabrication de produits allonges finis a chaud, notamment du type barre ou tube, en acier fortement allie ou hypereutectoide Download PDF

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Publication number
EP0820529B1
EP0820529B1 EP96907260A EP96907260A EP0820529B1 EP 0820529 B1 EP0820529 B1 EP 0820529B1 EP 96907260 A EP96907260 A EP 96907260A EP 96907260 A EP96907260 A EP 96907260A EP 0820529 B1 EP0820529 B1 EP 0820529B1
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European Patent Office
Prior art keywords
temperature
process according
deformation
rolling
cooling
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Expired - Lifetime
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EP96907260A
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German (de)
English (en)
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EP0820529A1 (fr
Inventor
Heinz Kron
Karlheinz Kutzenberger
Günther Manig
Gustav Zouhar
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.)
Vodafone GmbH
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Mannesmann AG
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Publication date
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Publication of EP0820529A1 publication Critical patent/EP0820529A1/fr
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Classifications

    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • 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
    • C21D1/26—Methods of annealing
    • C21D1/32—Soft annealing, e.g. spheroidising
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C21D8/065—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/003—Cementite
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr

Definitions

  • the invention relates to a method for producing a hot-made elongated product, in particular rod or tube made of high alloy or hypereutectoid steel according to the generic concept of the main claim.
  • High-alloy or hypereutectic steels especially rolling bearing steel such as B. 100Cr6 form when cooling from high temperatures (1100 to 1250 ° C) Grain boundary carbides and pearlitic structural components. These worsen one mechanical workability and hardenability as well as non-cutting forming.
  • the Suitable structures with spherical cementite can only be processed after long annealing processes (GKZ annealing) of 16 hours and more can be set. There have been a lot of considerations in the past on how to do this Shorten the duration of the soft annealing or even completely replace the soft annealing can.
  • thermomechanically treated structure shows such a finely dispersed distribution of the carbides that the limits of the resolving power of the light microscope are reached.
  • the more favorable distribution is justified by an increase in the dislocation density and the sub-grain boundaries resulting from the dislocations, which creates new nucleation sites for the carbides.
  • From DE-PS 2361330 is a process for the production of cylindrical Rolling elements made of steel with 0.7 to 1.2 mass percent in percent carbon known.
  • the steel wire hot-rolled at 1000 ° C quickly becomes cooled to a temperature corresponding to its lower pearlite level, then isothermally converted and hardness by cold drawing without intermediate annealing brought by 50 HRC.
  • the rapid cooling of the wire as well as the Subsequent isothermal transformation becomes a structure with fine lamellar pearlite achieved, which makes it possible to close the wire after descaling and phosphating pull without the need for an intermediate annealing.
  • the object of the present invention is a particularly inexpensive method for the production of a hot-formed elongated product in particular Rod or tube made of high-alloy steel or hypereutectoid steel in particular Rolling steel to specify, in which a structure is created that without a previous one Soft annealing such as B. Annealing on spherical cementite (GKZ) for a chipless Further processing and a final heat treatment is very suitable.
  • Another The task is to create a structure that is without a previous one Soft annealing for subsequent machining with a final one Final heat treatment is also suitable.
  • the coordinated process steps make it possible to produce the desired structure, with a Brinell hardness of less than or equal to 280 HB30, preferably less than 250 HB30, being achieved in the case of rolling bearing steel.
  • This structure also makes it possible, for example, to supply hot-worked pipes directly to processing without soft annealing.
  • the optimized manufacturing process is particularly cost-effective because the soft annealing and the associated transport and work steps are eliminated.
  • the processing of the elongated products which are hot-produced according to the invention can be cold drawing or cold vocationalage or cold rolls or transverse rolls. The method steps which contribute significantly to the success of the method according to the invention are explained in detail below.
  • a first process step is the controlled heating or cooling in the sense of temperature compensation over the length and extent of the rolling stock having a different temperature, the controlled compensation temperature being below the predetermined temperature in the reheating furnace.
  • the above-mentioned measure has the purpose, on the one hand, of being able to set the temperature of the rolling stock very precisely, taking into account the control options of the reheating furnace. Furthermore, this measure is intended to ensure that the most exact and reproducible conditions are possible for the temperature-dependent measurement of the wall thickness in the pipe before it enters the reducing mill.
  • the measure to be taken, ie heating or cooling, depends on the thickness of the material to be rolled.
  • the temperature of the tube after the first forming, punching, elongation and impacting will be above 700 ° C.
  • temperature compensation is achieved by controlled cooling to a predetermined compensation temperature in a temperature range between 650 ° and 700 ° C.
  • the temperature is frequently below 650 ° so that the temperature compensation must then take place via controlled heating to a predetermined compensation temperature in the previously mentioned range between 650 and 700 ° C.
  • the Ac 1 or Ac ma temperature is primarily dependent on the carbon content of the material quality used and on the forming history.
  • the former temperature range corresponds to the two-phase region ⁇ + Fe 3 C in the continuous time-temperature conversion diagram (ZTU), the latter to the two-phase region ⁇ + Fe 3 C.
  • Another measure for the proposed combination of coordinated process steps relates to the final continuous rolling process, preferably in the stretch-reducing mill.
  • the intervention possibilities in this fast-running continuous rolling process are low.
  • it is important for the proposed method that, on the one hand, a minimum partial deformation per extension in the reducing mill is expressed as the elongation ⁇ RW ⁇ 1.03 and, on the other hand, a minimum degree of elongation for the total deformation ⁇ ⁇ 1.5.
  • the total stretch can even be somewhat lower, ie ⁇ ⁇ 1.4.
  • the temperature increase resulting during the rolling due to the dissipation work or a temperature drop resulting due to excessive cooling should be as small as possible.
  • the method according to the invention is generally known for all Pipe production processes applicable, which end up with a reduction mill or without train or sizing mill.
  • this can be a procedure a Rohrkonti Avenue, Stopfen Avenue or an Asselwalzwerk. All it is particularly suitable for the push bench process for the production of seamless tubes Rolling steel suitable.
  • a feedstock for the process of the invention block casting (forged or rolled) or continuous casting (square or round) come in Question, the continuous casting material in a known manner before rolling use is deformed and annealed.
  • the method is special is to be used advantageously if the chemical analysis of the known Rolling steel is modified. This affects the sulfur and Phosphorus content and on the other hand the ratio of chromium to carbon.
  • the sulfur and phosphorus content should not exceed 0.005 percent by mass amount to possible melting at the grain boundaries with increasing Forming speed taking into account the ratio of manganese to Avoid sulfur by suppressing FeS. This is a risk of melting through the required high forming temperature in the first forming steps given when the strain rates are such that they become one lead to a corresponding temperature increase. For this reason, the The rate of deformation in the first forming stages was chosen so that the Temperature inside the rolling stock, d. H. not at the worst point 1170 ° C exceeds. In addition, low levels of S and P may have a beneficial effect following chipless forming processes.
  • the lowered S and P levels are also beneficial in secondary metallurgy to set a low oxygen content in the melt, which leads to a Improvement in the oxide purity leads.
  • the chromium to carbon ratio is said to be in the range between 1.35 and 1.52 preferably 1.45.
  • the carbon content is then, for example, 0.94 Mass fractions in percent and the chromium content about 1.36 mass fractions in percent. This ratio can have a positive effect on the undesired carbide rate become.
  • Another improvement is the cooling process after the last one Forming process.
  • the rolling stock After leaving the rolling mill, the rolling stock is in still air or cooled to a temperature by means of an air shower, which is shown in the ZTU diagram corresponds to a structure above the martensite point and below the nose of the bainite.
  • the formed material is isothermal for several hours in this area held.
  • This practice has been aimed at reducing the Internal stresses found to be favorable. This can be done in the way take place that the cooling bed at a suitable location, for example, insulating covered or the rolling stock is fed to a temperature compensation or tempering furnace becomes.
  • a hot tube of 40.9 mm outer diameter x 4.8 mm wall thickness made of 100Cr6 is to be produced on a pipe ram bench system.
  • Insert blocks with a length of approx. 850 mm are cut from a continuous casting rod with a diameter of 220 mm and a length of 11000 mm.
  • the 100Cr6 insert blocks are in the as-cast state, ie they are neither heat-treated nor pre-deformed.
  • the cut blocks are placed in a rotary hearth furnace and heated to approx. 1140 ° C. After a total heating time of 150 minutes, the blocks are removed individually from the furnace and, after descaling the press water, fed to the punch press.
  • the first forming into a perforated piece takes place in the punch press.
  • the hole piece has the following dimensions Outside diameter 223 mm Inner diameter 121 mm Wall thickness 51 mm.
  • the strain rate in this example is 0.45 s -1 and affects the optimal temperature window.
  • Another punching process follows the punch press, namely elongation in a shoulder mill. This deformation creates a sleeve with an outer diameter of 192 mm, an inner diameter of 112 mm and a wall thickness of 40 mm.
  • the third forming step is followed by bumping on the push bench.
  • a bench bench blank is manufactured with an outside diameter of 122.8 mm, an inside diameter of 112 mm and a wall thickness of 5.4 mm. After pushing through a number of stands, the blanks are released from the rod as an internal tool in a release roller mill.
  • the temperature of the slug drops further until the pull-out duo and in the aforementioned case reaches a level in the range of 650 to 700 ° C. After pulling out the bumper, the slug bottom is scooped.
  • the slug bottom is scooped prior to the entry of the slug into the reheating device.
  • it is subjected to controlled cooling in order to achieve a uniform temperature distribution in the range between 650 ° C. and 700 ° C.
  • a temperature level of approx. 670 ° C is aimed for.
  • the slugs are held for a certain time by means of a heat-insulated buffer, so that heat can flow from the areas of the slug with a higher temperature level to the areas with a low temperature level.
  • the thermal insulation ensures that the overall level of the bobbin temperature does not drop below the specified target value.
  • the temperature of the reheating furnace is set so that the temperature of the material to be formed is approximately 740 ° C.
  • the billet enters a stretch-reducing mill. This consists of a large number of three-roll stands, which are each offset by 120 ° in a rolling line. 19 frames are used for the selected example with the final dimensions of 40.9 x 4.8 mm.
  • the partial forming in the basic scaffolding is estimated to be between 7.1 and 8.1% decrease in cross-section. The total deformation is 72.7% corresponding to an elongation ⁇ of 3.66.
  • the forming conditions are chosen such.
  • the tube made of 100Cr6 rolled in this way has, after cooling, a structure that approximates the GKZ structure.
  • the finely dispersed structure consists of molded cementite with minor pearlite residues.
  • the Brinell hardness of the tube thus produced is less than 250 HB30.
  • the spread of hardness values is low.
  • the structure is finer than after conventional GKZ annealing as the comparison of Figure 1 with Figure 2 shows.
  • the same final dimension is 40.9 mm outer Diameter x 4.8 mm wall thickness made of 100Cr6 also rolled in the usual way been.
  • the hardness determined on these tubes is 328 HB30 with one adjustment of the reheating oven to 1000 ° C. This hardness is so high that before a Further processing a GKZ annealing is required.
  • the cooling according to the ZTU diagram is advantageous to control the cooling according to the ZTU diagram so that above the martensite point but below the bainite nose isothermal Hold time is introduced.
  • the temperature range is preferably between 240 and 300 ° C. After holding in this temperature area for more than 3.5 hours can be cooled to room temperature.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Heat Treatment Of Steel (AREA)
  • Metal Rolling (AREA)
  • Metal Extraction Processes (AREA)

Claims (10)

  1. Procédé pour fabriquer un produit allongé préparé à chaud, en particulier une barre ou un tube en acier fortement allié ou hypereutectoïde, dans lequel la longueur de la matière de départ choisie, chauffée à la température de déformation, est à nouveau chauffée après une ou plusieurs étapes de déformation à une température se trouvant au-dessous de la température de déformation initiale et est déformée à la dimension finale par un laminage continu au moyen d'un laminoir réducteur à plusieurs cages et, ensuite, refroidie à l'air statique,
    caractérisé en ce que, après les premières étapes de déformation et avant le réchauffage, il est engendré une répartition de température uniforme, relativement à la longueur et à l'épaisseur du produit intermédiaire, à l'intérieur d'une plage de température déterminée, par un chauffage ou refroidissement réglé à une température prédéfinie, et le réchauffage suivant est effectué à une température soit au-dessous de Aci mais supérieure à 650° C, soit au-dessus de Aci mais inférieure à Acma dans le domaine à deux phases, et la déformation et le refroidissement, ainsi que le chauffage extérieur le cas échéant supplémentaire, sont réglés dans le laminoir réducteur de sorte que l'augmentation de la température dans la matière laminée demeure faible relativement à la température de passe initiale, et la matière laminée, pendant la déformation dans le laminoir réducteur et lorsqu'elle quitte le laminoir, se trouve, relativement à la température, dans le domaine à deux phases, la déformation minimale exprimée comme allongement valant, pour la déformation globale, λ ≥ 1,5 et, pour la déformation partielle minimale dans la cage individuelle du laminoir réducteur, λRW ≥ 1,03.
  2. Procédé selon la revendication 1,
    caractérisé en ce que la température prédéfinie pour la compensation de température avant le réchauffage se trouve dans une plage entre 650° C et 700° C.
  3. Procédé selon les revendications 1 et 2,
    caractérisé en ce que le réchauffage de la matière laminée est effectué à une température dans une plage supérieure à 650° C mais inférieure à 710° C ou dans une plage de température supérieure à 710° C mais inférieure à 880° C.
  4. Procédé selon les revendications 1 à 3,
    caractérisé en ce que l'augmentation de température ou la chute de température de la matière laminée dans le laminoir réducteur est maintenue dans d'étroites limites par l'intermédiaire d'une régulation du fluide de refroidissement commandée, dans des cas particuliers une amenée de chaleur au moyen d'un dispositif thermique externe, ainsi que par l'intermédiaire de la variation de la géométrie de laminage, de la vitesse de laminage et de la réduction aux différentes passes.
  5. Procédé selon les revendications 1 à 4,
    caractérisé en ce que, lorsque l'on utilise un acier hypereutectoïde, en particulier de l'acier pour paliers à roulements, la teneur en soufre et en phosphore vaut au maximum, à chaque fois, 0,005 en pourcentage massique et une plage entre 1,35 et 1,52 est choisie pour le rapport chrome-carbone.
  6. Procédé selon la revendication 5,
    caractérisé en ce que le rapport Cr/C vaut avantageusement 1,45.
  7. Procédé selon les revendications 1 à 6,
    caractérisé en ce que, comme matière de départ, on utilise une barre de coulée continue sans une quelconque déformation préalable, c'est-à-dire dans l'état de coulée et sans traitement thermique préalable (recuit de diffusion).
  8. Procédé selon les revendications 1 à 7,
    caractérisé en ce que la vitesse de modification de forme, dans les premières étapes de déformation avant la compensation de température, est choisie de sorte que la température la plus élevée à l'intérieur de la matière laminée ne dépasse pas 1170° C.
  9. Procédé selon les revendications 1 à 8,
    caractérisé en ce que la matière laminée est refroidie après le laminage à une température au-dessus de la température martensitique et au-dessous du bec de bainite (diagramme ZTU continu) et maintenue un temps plus long, et, ensuite, est refroidie, de façon connue, jusqu'à la température ambiante.
  10. Procédé selon les revendications 1 à 9,
    caractérisé en ce que le produit laminé fini est chauffé, après le refroidissement, à une température entre 650 et 700° C et maintenu pendant un temps prédéfini et, ensuite, est à nouveau refroidi et, alors, un revenu est effectué à une température entre 180 et 210° C avec refroidissement suivant à l'air statique.
EP96907260A 1995-04-03 1996-03-12 Procede de fabrication de produits allonges finis a chaud, notamment du type barre ou tube, en acier fortement allie ou hypereutectoide Expired - Lifetime EP0820529B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19513314 1995-04-03
DE19513314A DE19513314C2 (de) 1995-04-03 1995-04-03 Verfahren zur Herstellung eines warmgefertigten langgestreckten Erzeugnisses, insbesondere Stab oder Rohr, aus übereutektoidem Stahl
PCT/DE1996/000501 WO1996031628A1 (fr) 1995-04-03 1996-03-12 Procede de fabrication de produits allonges finis a chaud, notamment du type barre ou tube, en acier fortement allie ou hypereutectoide

Publications (2)

Publication Number Publication Date
EP0820529A1 EP0820529A1 (fr) 1998-01-28
EP0820529B1 true EP0820529B1 (fr) 2000-08-02

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EP96907260A Expired - Lifetime EP0820529B1 (fr) 1995-04-03 1996-03-12 Procede de fabrication de produits allonges finis a chaud, notamment du type barre ou tube, en acier fortement allie ou hypereutectoide

Country Status (14)

Country Link
US (1) US5958158A (fr)
EP (1) EP0820529B1 (fr)
JP (1) JPH11503491A (fr)
KR (1) KR19980703575A (fr)
AR (1) AR001416A1 (fr)
BR (1) BR9604830A (fr)
CA (1) CA2217309C (fr)
CZ (1) CZ304797A3 (fr)
DE (2) DE19513314C2 (fr)
ES (1) ES2149455T3 (fr)
HU (1) HUP9800702A3 (fr)
PL (1) PL322598A1 (fr)
SK (1) SK134297A3 (fr)
WO (1) WO1996031628A1 (fr)

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SE9800860L (sv) * 1998-03-16 1999-05-25 Ovako Steel Ab Sätt för mjukglödgning av högkolhaltigt stål
NL1007739C2 (nl) * 1997-12-08 1999-06-09 Hoogovens Staal Bv Werkwijze en inrichting voor het vervaardigen van een stalen band met hoge sterkte.
US6233500B1 (en) * 1997-06-19 2001-05-15 The United States Of America As Represented By The Secretary Of The Air Force Optimization and control of microstructure development during hot metal working
DE19734563C1 (de) * 1997-08-04 1998-12-03 Mannesmann Ag Verfahren zur Herstellung von Wälzlagerringen aus Stahl
DE10134776C2 (de) * 2000-07-12 2003-04-24 Mannesmann Roehren Werke Ag Verfahren zur Herstellung metallischer nicht-rotationssymmetrischer Ringe mit über den Umfang konstanter Wanddicke, sowie Vorrichtung zur Durchführung des Verfahrens
US6936119B2 (en) * 2000-07-12 2005-08-30 Mannesmannrohren-Werke Ag Method for producing metallic, non-rotationally symmetrical rings with a constant wall thickness over their circumference
DE102004011021A1 (de) * 2004-03-04 2005-09-29 Mannesmannröhren-Werke Ag Verfahren zur Herstellung eines Formteils aus übereutekoidem Stahl
JP4894855B2 (ja) 2006-03-28 2012-03-14 住友金属工業株式会社 継目無管の製造方法
US9132567B2 (en) * 2007-03-23 2015-09-15 Dayton Progress Corporation Tools with a thermo-mechanically modified working region and methods of forming such tools
US8968495B2 (en) * 2007-03-23 2015-03-03 Dayton Progress Corporation Methods of thermo-mechanically processing tool steel and tools made from thermo-mechanically processed tool steels
CN101722190B (zh) * 2009-11-12 2012-08-22 无锡西姆莱斯石油专用管制造有限公司 一种热轧毛管的处理工艺
DE102011051682B4 (de) * 2011-07-08 2013-02-21 Max Aicher Verfahren und Vorrichtung zum Behandeln eines Stahlprodukts sowie Stahlprodukt
PL232555B1 (pl) * 2017-05-25 2019-06-28 Arcelormittal Poland Spolka Akcyjna Sposób produkcji walcówki gładkiej i żebrowanej

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JPS6417820A (en) * 1987-07-13 1989-01-20 Kobe Steel Ltd Production of electric resistance welded steel tube for heat treatment
JP3215891B2 (ja) * 1991-06-14 2001-10-09 新日本製鐵株式会社 冷間加工用棒鋼線材の製造方法
JP2544867B2 (ja) * 1992-04-21 1996-10-16 新日本製鐵株式会社 過共析鋼線材の製造方法
EP0586335B1 (fr) * 1992-09-02 2000-05-03 Sulzer Orthopädie AG Coque acétubulaire en deux parties

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Publication number Publication date
KR19980703575A (ko) 1998-11-05
CZ304797A3 (cs) 1998-04-15
SK134297A3 (en) 1998-04-08
DE19513314C2 (de) 1997-07-03
ES2149455T3 (es) 2000-11-01
WO1996031628A1 (fr) 1996-10-10
AR001416A1 (es) 1997-10-22
JPH11503491A (ja) 1999-03-26
DE19513314A1 (de) 1996-10-10
PL322598A1 (en) 1998-02-02
HUP9800702A2 (hu) 1998-07-28
CA2217309A1 (fr) 1996-10-10
EP0820529A1 (fr) 1998-01-28
CA2217309C (fr) 2000-11-21
US5958158A (en) 1999-09-28
DE59605681D1 (de) 2000-09-07
HUP9800702A3 (en) 1999-08-30
BR9604830A (pt) 1999-01-05

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