US20020011284A1 - Method for making seamless tubing with a stable elastic limit at high application temperatures - Google Patents

Method for making seamless tubing with a stable elastic limit at high application temperatures Download PDF

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Publication number
US20020011284A1
US20020011284A1 US09/341,722 US34172299A US2002011284A1 US 20020011284 A1 US20020011284 A1 US 20020011284A1 US 34172299 A US34172299 A US 34172299A US 2002011284 A1 US2002011284 A1 US 2002011284A1
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Prior art keywords
max
steel
pipes
temperature
hot
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Abandoned
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US09/341,722
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Ingo von Hagen
Markus Ring
Gerd Heinz
Bernhard Koschlig
Kurt Niederhoff
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Vodafone GmbH
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Mannesmann AG
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Assigned to MANNESMANN AG reassignment MANNESMANN AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HEINZ, GERD, KOSCHLIG, BERNHARD, NIEDERHOFF, KURT, RING, MARKUS, VON HAGEN, INGO
Publication of US20020011284A1 publication Critical patent/US20020011284A1/en
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    • 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
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • 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
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • 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

Definitions

  • the invention relates to a process for producing seamless line pipes within the quality grade range X 52 to X 90.
  • tungsten As an alloying element, it is regularly used to produce cold-work, hot-work and high-speed steels. It increases their high-temperature strength, ability to withstand tempering and, in particular, the wear resistance at high temperatures. Tungsten acts in a similar way to molybdenum, so that it can replace molybdenum in a ratio of 2:1.
  • ferritic alloys containing 9 to 12% chromium which are able to withstand high temperatures are used for steam pipelines.
  • Examples of such steels are the alloys P 92 and P 122 from Japan and the European-developed material E 911.
  • the object of the invention is to propose a method for the production of seamless line pipes, in which method it is possible to reliably set a quality grade in the range from X 52 to X 90 by means of a quenching and tempering treatment and to ensure a stable yield strength combined with an essentially constant stress-strain characteristic up to temperatures of use of 200° C.
  • this object is achieved by hot-rolling of a pipe blank made from a steel of the following composition (% by weight): C 0.06-0.18% Si max. 0.40% Mn 0.80-1.40% P max. 0.025% S max. 0.010% Al 0.010-0.060% Mo max. 0.50% V max. 0.10% Nb max. 0.10% N max. 0.015% W >0.30-1.00%
  • the nitrogen content it is recommended to add up to 0.050% Ti to the steel alloy used.
  • the tungsten content expediently lies in the range from 0.35 to 0.70%, particularly preferably in the range from 0.35 to 0.40%. It is recommended to set the vanadium content at at least 0.04%.
  • the steel alloy which is to be used for the hot rolling according to the invention may perfectly well contain further accompanying substances, such as those which are used in particular for electric-furnace steelmaking, without its properties being impaired.
  • accompanying substances are copper, chromium and nickel.
  • the steel should contain at most 0.15% of each of these accompanying substances.
  • a line pipe which has been hot-rolled and quenched after reheating according to the invention can be set at any desired quality grade within the range from X 52 to X 90 by means of quenching and tempering.
  • the toughness properties are improved by increasing the tempering temperatures.
  • a line pipe which is produced according to the invention has a stable yield strength at least up to a temperature of use of 200° C., i.e. the reduction in yield strength is very low ( ⁇ 10%).
  • the stress-strain characteristic is essentially constant.
  • the weldability, which is important for line pipes, is guaranteed.
  • the carbon equivalent according to IIW can be set at relatively low levels.
  • the molybdenum content can be limited to very low values or may even be zero. Since tungsten is less expensive than molybdenum, the alloy which is to be used according to the invention costs less to produce.
  • the carbon equivalent values for the comparison steel were 0.44 and 0.24, respectively.
  • the alloy of the steel used according to the invention differs from the comparison alloy essentially only in that the molybdenum content is 0.15% lower, and an additional content of 0.35% tungsten is added instead.
  • the yield strength of the steel used according to the invention fell by only approx. 5%.
  • the stress-strain characteristic in FIG. 1 surprisingly the stress-strain curves at room temperature (RT) and at the test temperature of 160° C.
  • the use of higher tempering temperatures makes it possible to reduce the strength level, while lower temperatures increase the strength level.
  • Within the limits of the alloying ranges according to the invention it is possible to select alloys which, by means of appropriate quenching and tempering treatment, can produce the quality grade range from X 52 to X 90. In terms of the notched-impact strength at a test temperature of ⁇ 30° C.
  • the tested steel specimen according to the invention achieved a notched-impact energy value of 92 J/cm 2 , which is regarded as extremely good for the quality grade X 85.
  • the weldability of the steel according to the invention can be classified as entirely satisfactory, and there is no evidence of the addition of tungsten to the alloy having any adverse effect.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)
  • Heat Treatment Of Articles (AREA)

Abstract

The invention relates to a process for producing seamless line pipes within the quality grade range X 52 to X 90, with a stable yield strength up to a temperature of use of 200° C., and with an essentially constant stress-strain characteristic, by hot-rolling a pipe blank made from a steel which contains the following alloying elements (% by weight): C 0.06-0.18% Si max. 0.40% Mn 0.80-1.40% P max. 0.025% S max. 0.010% Al 0.010-0.060% Mo max. 0.50% V max. 0.10% Nb max. 0.10% N max. 0.015% W >0.30-1.00%
remainder iron and usual impurities, in which process the hot rolling is followed by reheating of the cooled pipes to above AC3, after which the pipes are quenched to below 100° C. at a cooling rate of at least 15° C./s and are then tempered within the temperature range from 500 to 700° C.

Description

    DESCRIPTION
  • The invention relates to a process for producing seamless line pipes within the quality grade range X 52 to X 90. [0001]
  • In the course of the exploration of deposits of hydrocarbons, deposits are increasingly being discovered which are difficult to convey owing to the fact that the hydrocarbons (e.g. natural gas) are at relatively high temperatures of, for example, from 100 to 200° C. The materials which can be used for line pipes under such conditions not only have to be sufficiently weldable and to have a certain resistance to corrosion, but also have to have a comparatively stable yield strength. For example, the reduction in yield strength at a temperature of 160° C. compared to the yield strength at room temperature should be as low as possible. Furthermore, an essentially constant stress-strain characteristic is required, i.e. the so-called Luders strain should be as low as possible. [0002]
  • It is generally relatively rare to use tungsten as an alloying element. As a strong carbide-forming element, it is regularly used to produce cold-work, hot-work and high-speed steels. It increases their high-temperature strength, ability to withstand tempering and, in particular, the wear resistance at high temperatures. Tungsten acts in a similar way to molybdenum, so that it can replace molybdenum in a ratio of 2:1. [0003]
  • In modern power plant construction, ferritic alloys containing 9 to 12% chromium which are able to withstand high temperatures are used for steam pipelines. For these steels, it is known to add from 1 to 2% tungsten to the alloy in order to increase the creep rupture strength. Examples of such steels are the alloys P 92 and P 122 from Japan and the European-developed material E 911. [0004]
  • Hitherto, there has been no knowledge whatsoever of using tungsten as an alkalyne element for line pipe steels. [0005]
  • The object of the invention is to propose a method for the production of seamless line pipes, in which method it is possible to reliably set a quality grade in the range from X 52 to X 90 by means of a quenching and tempering treatment and to ensure a stable yield strength combined with an essentially constant stress-strain characteristic up to temperatures of use of 200° C.[0006]
  • According to the invention, this object is achieved by hot-rolling of a pipe blank made from a steel of the following composition (% by weight): [0007]
    C 0.06-0.18%
    Si max. 0.40%
    Mn 0.80-1.40%
    P max. 0.025%
    S max. 0.010%
    Al 0.010-0.060%
    Mo max. 0.50%
    V max. 0.10%
    Nb max. 0.10%
    N max. 0.015%
    W >0.30-1.00%
  • remainder iron and usual impurities. [0008]
  • Following the hot rolling and cooling of the pipes, they are reheated to a temperature above AC[0009] 3 and quenched to below 100° C. at a cooling rate of at least 15° C./s. Then, the pipes are tempered within the temperature range from 500 to 700° C., depending on the quality grade desired.
  • In many cases, for fixation of the nitrogen content, it is recommended to add up to 0.050% Ti to the steel alloy used. The tungsten content expediently lies in the range from 0.35 to 0.70%, particularly preferably in the range from 0.35 to 0.40%. It is recommended to set the vanadium content at at least 0.04%. A molybdenum content in the range from 0.05 to 0.40%, preferably in the range from 0.10 to 0.25%, has proven advantageous particularly for the higher quality grades. [0010]
  • The steel alloy which is to be used for the hot rolling according to the invention may perfectly well contain further accompanying substances, such as those which are used in particular for electric-furnace steelmaking, without its properties being impaired. Examples of such accompanying substances are copper, chromium and nickel. Expediently, the steel should contain at most 0.15% of each of these accompanying substances. [0011]
  • A line pipe which has been hot-rolled and quenched after reheating according to the invention can be set at any desired quality grade within the range from X 52 to X 90 by means of quenching and tempering. The lower the tempering temperature selected, the higher the strength characteristics which can be achieved. The toughness properties are improved by increasing the tempering temperatures. A line pipe which is produced according to the invention has a stable yield strength at least up to a temperature of use of 200° C., i.e. the reduction in yield strength is very low (<10%). The stress-strain characteristic is essentially constant. The weldability, which is important for line pipes, is guaranteed. The carbon equivalent according to IIW can be set at relatively low levels. The molybdenum content can be limited to very low values or may even be zero. Since tungsten is less expensive than molybdenum, the alloy which is to be used according to the invention costs less to produce. [0012]
  • The important addition of tungsten to the alloy, which is the decisive factor for the invention, has produced a positive effect which is surprising to the person skilled in the art. This is to be illustrated below using an exemplary embodiment and a comparative example. The stress-strain characteristic of specimens of the two examples is illustrated in graphs in FIG. 1 (invention) and FIG. 2 (comparison). [0013]
  • Tests were carried out on test specimens with a thickness of 35 mm in each case, which had been rolled in a pilger-rolling mill train. The alloys used for the two examples are given in the following table: [0014]
    Element Invention Comparison
    C 0.13% 0.13%
    Mn 1.30% 1.25%
    Mo 0.15% 0.30%
    V 0.05% 0.05%
    Cr 0.10% 0.10%
    W 0.35% —
    Ti 0.018% 0.018%
    N 70 ppm 70 ppm
  • For the steel used according to the invention, the carbon equivalent was determined to have the value TE[0015] IIW=0.42 or CEPCM=0.23. The carbon equivalent values for the comparison steel were 0.44 and 0.24, respectively. The alloy of the steel used according to the invention differs from the comparison alloy essentially only in that the molybdenum content is 0.15% lower, and an additional content of 0.35% tungsten is added instead. During the testing of the strength properties at a test temperature of 160° C., the yield strength of the steel used according to the invention fell by only approx. 5%. As can be seen from the stress-strain characteristic in FIG. 1, surprisingly the stress-strain curves at room temperature (RT) and at the test temperature of 160° C. coincide virtually completely beyond a plastic extension of approx. 0.7%. By comparison, the similar stress-strain diagram for the molybdenum-alloyed comparison steel which is illustrated in FIG. 2 reveals a very different behavior. In this case, the stress-strain curve at the test temperature of 160° C. lies significantly below the stress-strain curve at room temperature over the entire range tested. This stress-strain performance of the line pipe steel used according to the invention, which is comparatively much more advantageous, was completely unexpected.
  • At a tempering temperature of 670° C., the tested specimen of the steel according to the invention had a yield strength of R[0016] p0.2=594 MPa, thus achieving the level of quality grade X 85. The use of higher tempering temperatures makes it possible to reduce the strength level, while lower temperatures increase the strength level. Within the limits of the alloying ranges according to the invention, it is possible to select alloys which, by means of appropriate quenching and tempering treatment, can produce the quality grade range from X 52 to X 90. In terms of the notched-impact strength at a test temperature of −30° C. (specimen position: center of sheet, transverse), the tested steel specimen according to the invention achieved a notched-impact energy value of 92 J/cm2, which is regarded as extremely good for the quality grade X 85. The weldability of the steel according to the invention can be classified as entirely satisfactory, and there is no evidence of the addition of tungsten to the alloy having any adverse effect.

Claims (5)

1. A process for producing seamless line pipes within the quality grade range X 52 to X 90, with a stable yield strength up to a temperature of use of 200° C., and with an essentially constant stress-strain characteristic, by hot-rolling a pipe blank made from a steel which contains the following alloying elements (% by weight):
C 0.06-0.18% Si max. 0.40% Mn 0.80-1.40% P max. 0.025% S max. 0.010% Al 0.010-0.060% Mo max. 0.50% V max. 0.10% Nb max. 0.10% N max. 0.015% W >0.30-1.00%
remainder iron and usual impurities, in which process the hot rolling is followed by reheating of the cooled pipes to above AC3, after which the pipes are quenched to below 100° C. at a cooling rate of at least 15° C./s and are then tempered within the temperature range from 500 to 700° C.
2. The process as claimed in claim 1, wherein up to 0.050% Ti is added to the steel which is to be used, for fixation of nitrogen.
3. The process as claimed in one of claims 1 to 2, wherein the steel which is to be used contains from 0.35 to 0.70%, in particular from 0.35 to 0.40%, W.
4. The process as claimed in one of claims 1 to 3, wherein the steel which is to be used contains from 0.05 to 0.40%, in particular from 0.10 to 0.25%, Mo.
5. The process as claimed in one of claims 1 to 4, wherein the steel which is to be used contains at least 0.04% V.
US09/341,722 1997-01-15 1997-12-12 Method for making seamless tubing with a stable elastic limit at high application temperatures Abandoned US20020011284A1 (en)

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DE19702823.3 1997-01-15

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US20080314481A1 (en) * 2005-08-04 2008-12-25 Alfonso Izquierdo Garcia High-Strength Steel for Seamless, Weldable Steel Pipes
US20100068549A1 (en) * 2006-06-29 2010-03-18 Tenaris Connections Ag Seamless precision steel tubes with improved isotropic toughness at low temperature for hydraulic cylinders and process for obtaining the same
US20100136363A1 (en) * 2008-11-25 2010-06-03 Maverick Tube, Llc Compact strip or thin slab processing of boron/titanium steels
US20100193085A1 (en) * 2007-04-17 2010-08-05 Alfonso Izquierdo Garcia Seamless steel pipe for use as vertical work-over sections
US20100294401A1 (en) * 2007-11-19 2010-11-25 Tenaris Connections Limited High strength bainitic steel for octg applications
US8002910B2 (en) 2003-04-25 2011-08-23 Tubos De Acero De Mexico S.A. Seamless steel tube which is intended to be used as a guide pipe and production method thereof
US8328958B2 (en) 2007-07-06 2012-12-11 Tenaris Connections Limited Steels for sour service environments
US8414715B2 (en) 2011-02-18 2013-04-09 Siderca S.A.I.C. Method of making ultra high strength steel having good toughness
US8636856B2 (en) 2011-02-18 2014-01-28 Siderca S.A.I.C. High strength steel having good toughness
US8821653B2 (en) 2011-02-07 2014-09-02 Dalmine S.P.A. Heavy wall steel pipes with excellent toughness at low temperature and sulfide stress corrosion cracking resistance
US9187811B2 (en) 2013-03-11 2015-11-17 Tenaris Connections Limited Low-carbon chromium steel having reduced vanadium and high corrosion resistance, and methods of manufacturing
US9340847B2 (en) 2012-04-10 2016-05-17 Tenaris Connections Limited Methods of manufacturing steel tubes for drilling rods with improved mechanical properties, and rods made by the same
US9598746B2 (en) 2011-02-07 2017-03-21 Dalmine S.P.A. High strength steel pipes with excellent toughness at low temperature and sulfide stress corrosion cracking resistance
US9644248B2 (en) 2013-04-08 2017-05-09 Dalmine S.P.A. Heavy wall quenched and tempered seamless steel pipes and related method for manufacturing said steel pipes
US9657365B2 (en) 2013-04-08 2017-05-23 Dalmine S.P.A. High strength medium wall quenched and tempered seamless steel pipes and related method for manufacturing said steel pipes
US9803256B2 (en) 2013-03-14 2017-10-31 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
US9970242B2 (en) 2013-01-11 2018-05-15 Tenaris Connections B.V. Galling resistant drill pipe tool joint and corresponding drill pipe
US10844669B2 (en) 2009-11-24 2020-11-24 Tenaris Connections B.V. Threaded joint sealed to internal and external pressures
US11105501B2 (en) 2013-06-25 2021-08-31 Tenaris Connections B.V. High-chromium heat-resistant steel
US11124852B2 (en) 2016-08-12 2021-09-21 Tenaris Coiled Tubes, Llc Method and system for manufacturing coiled tubing
US11833561B2 (en) 2017-01-17 2023-12-05 Forum Us, Inc. Method of manufacturing a coiled tubing string
US11952648B2 (en) 2011-01-25 2024-04-09 Tenaris Coiled Tubes, Llc Method of forming and heat treating coiled tubing

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DE19942641A1 (en) * 1999-08-30 2001-03-22 Mannesmann Ag Use of a steel alloy for the production of high-strength seamless steel pipes
CN102127698A (en) * 2011-02-22 2011-07-20 中国石油天然气集团公司 Production method of X100 steel grade elbow pipes and pipe fittings
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CA1249121A (en) * 1983-06-13 1989-01-24 Tadaaki Taira Method for manufacturing bent steel pipe excellent in strength and low-temperature toughness
DE3832014C2 (en) * 1988-09-16 1994-11-24 Mannesmann Ag Process for the production of high-strength seamless steel tubes
DK0789785T3 (en) * 1994-11-04 2002-11-25 Babcock Hitachi Kk Ferritic heat resistant steel type with excellent high temperature strength and process for making it

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US8002910B2 (en) 2003-04-25 2011-08-23 Tubos De Acero De Mexico S.A. Seamless steel tube which is intended to be used as a guide pipe and production method thereof
US20080314481A1 (en) * 2005-08-04 2008-12-25 Alfonso Izquierdo Garcia High-Strength Steel for Seamless, Weldable Steel Pipes
US8007603B2 (en) 2005-08-04 2011-08-30 Tenaris Connections Limited High-strength steel for seamless, weldable steel pipes
US20100068549A1 (en) * 2006-06-29 2010-03-18 Tenaris Connections Ag Seamless precision steel tubes with improved isotropic toughness at low temperature for hydraulic cylinders and process for obtaining the same
US8926771B2 (en) 2006-06-29 2015-01-06 Tenaris Connections Limited Seamless precision steel tubes with improved isotropic toughness at low temperature for hydraulic cylinders and process for obtaining the same
US20100193085A1 (en) * 2007-04-17 2010-08-05 Alfonso Izquierdo Garcia Seamless steel pipe for use as vertical work-over sections
US8328958B2 (en) 2007-07-06 2012-12-11 Tenaris Connections Limited Steels for sour service environments
US20100294401A1 (en) * 2007-11-19 2010-11-25 Tenaris Connections Limited High strength bainitic steel for octg applications
US8328960B2 (en) 2007-11-19 2012-12-11 Tenaris Connections Limited High strength bainitic steel for OCTG applications
US8221562B2 (en) 2008-11-25 2012-07-17 Maverick Tube, Llc Compact strip or thin slab processing of boron/titanium steels
US20100136363A1 (en) * 2008-11-25 2010-06-03 Maverick Tube, Llc Compact strip or thin slab processing of boron/titanium steels
US10844669B2 (en) 2009-11-24 2020-11-24 Tenaris Connections B.V. Threaded joint sealed to internal and external pressures
US11952648B2 (en) 2011-01-25 2024-04-09 Tenaris Coiled Tubes, Llc Method of forming and heat treating coiled tubing
US8821653B2 (en) 2011-02-07 2014-09-02 Dalmine S.P.A. Heavy wall steel pipes with excellent toughness at low temperature and sulfide stress corrosion cracking resistance
US9598746B2 (en) 2011-02-07 2017-03-21 Dalmine S.P.A. High strength steel pipes with excellent toughness at low temperature and sulfide stress corrosion cracking resistance
US8414715B2 (en) 2011-02-18 2013-04-09 Siderca S.A.I.C. Method of making ultra high strength steel having good toughness
US9222156B2 (en) 2011-02-18 2015-12-29 Siderca S.A.I.C. High strength steel having good toughness
US9188252B2 (en) 2011-02-18 2015-11-17 Siderca S.A.I.C. Ultra high strength steel having good toughness
US8636856B2 (en) 2011-02-18 2014-01-28 Siderca S.A.I.C. High strength steel having good toughness
US9340847B2 (en) 2012-04-10 2016-05-17 Tenaris Connections Limited Methods of manufacturing steel tubes for drilling rods with improved mechanical properties, and rods made by the same
US9970242B2 (en) 2013-01-11 2018-05-15 Tenaris Connections B.V. Galling resistant drill pipe tool joint and corresponding drill pipe
US9187811B2 (en) 2013-03-11 2015-11-17 Tenaris Connections Limited Low-carbon chromium steel having reduced vanadium and high corrosion resistance, and methods of manufacturing
US9803256B2 (en) 2013-03-14 2017-10-31 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
US10378075B2 (en) 2013-03-14 2019-08-13 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
US10378074B2 (en) 2013-03-14 2019-08-13 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
US11377704B2 (en) 2013-03-14 2022-07-05 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
US9657365B2 (en) 2013-04-08 2017-05-23 Dalmine S.P.A. High strength medium wall quenched and tempered seamless steel pipes and related method for manufacturing said steel pipes
US9644248B2 (en) 2013-04-08 2017-05-09 Dalmine S.P.A. Heavy wall quenched and tempered seamless steel pipes and related method for manufacturing said steel pipes
US11105501B2 (en) 2013-06-25 2021-08-31 Tenaris Connections B.V. High-chromium heat-resistant steel
US11124852B2 (en) 2016-08-12 2021-09-21 Tenaris Coiled Tubes, Llc Method and system for manufacturing coiled tubing
US11833561B2 (en) 2017-01-17 2023-12-05 Forum Us, Inc. Method of manufacturing a coiled tubing string

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NO993260L (en) 1999-06-30
NO993260D0 (en) 1999-06-30
AU5748298A (en) 1998-08-07
JP2001508131A (en) 2001-06-19
EP0954617B1 (en) 2001-08-08
ES2159155T3 (en) 2001-09-16
WO1998031843A1 (en) 1998-07-23
EP0954617A1 (en) 1999-11-10
DE59704264D1 (en) 2001-09-13

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