EP0367360B1 - Process for manufacturing seamless pressure vessels - Google Patents

Process for manufacturing seamless pressure vessels Download PDF

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Publication number
EP0367360B1
EP0367360B1 EP89250061A EP89250061A EP0367360B1 EP 0367360 B1 EP0367360 B1 EP 0367360B1 EP 89250061 A EP89250061 A EP 89250061A EP 89250061 A EP89250061 A EP 89250061A EP 0367360 B1 EP0367360 B1 EP 0367360B1
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EP
European Patent Office
Prior art keywords
pressure vessels
strength
tempering
tempered
steel
Prior art date
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Expired - Lifetime
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EP89250061A
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German (de)
French (fr)
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EP0367360A2 (en
EP0367360A3 (en
Inventor
Dieter Dr.-Ing. Vespermann
Heinz Müller
Bernhard Dipl.-Ing. Hoffmann
Ingo Dr.-Ing. Von Hagen
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Vodafone GmbH
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Mannesmann AG
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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
    • C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
    • 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
    • C21D9/14—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes wear-resistant or pressure-resistant pipes
    • 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
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • 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
    • C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron

Definitions

  • the invention relates to a method for producing seamless pressure vessels from a CrMo steel according to the preamble of the patent claim.
  • Tempering is carried out at 530 to 680 ° C with a holding time of at least 2 min per mm wall thickness, but at least 30 min. and carried out with subsequent cooling in air.
  • the strict measurement value A2 is used.
  • the values for the 0.2 proof stress were scattered, the scattering range being 85 N / mm2. The same applies to the hardness, which was spread over a range of 40 HB.
  • the object of the invention is to improve a generic method for producing pressure vessels from a CrMo steel in such a way that an increase in the strength values or toughness properties is not associated with a corresponding deterioration in the other properties.
  • the mechanical-technological properties should be made more uniform.
  • microalloying elements Ti and B are associated with strengthening and toughening properties after tempering.
  • Example 2 aimed to increase the strength while largely maintaining the toughness properties.
  • values for the notched impact strength of 95 J / cm2 and 68 J / cm2 at -20 o C and -40 o C there were even improvements in toughness compared to the comparative example by about 9% and 31%;
  • the elongation A 2 ⁇ was 13.5%, only slightly below the minimum value of 14% required per se .
  • this impairment is easily tolerable against the background that the yield strength R p0.2 could be increased from 812 N / mm2 to 1025 N / mm2, ie by about 26%, without sacrificing toughness.
  • the spread of the yield strength and the hardness were reduced by 39% and 22%, respectively.

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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 Articles (AREA)
  • Heat Treatment Of Steel (AREA)
  • Press Drives And Press Lines (AREA)

Abstract

The invention relates to a process for manufacturing seamless pressure vessels from an aluminium-killed CrMo steel of specific composition. After hot forming, the pressure vessels are tempered by austenitising at 830 to 880 DEG C, cooling at a rate of 5 to 15 K/s to room temperature and drawing up to 680 DEG C and cooling in air. The steel alloy is distinguished by a nitrogen content of 0.003 to 0.01% and furthermore contains 0.010 to 0.040% of titanium and 0.001 to 0.03% of boron, with a Ti/N ratio of at least 3:4.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung nahtloser Druckbehälter aus einem CrMo-Stahl gemäß dem Oberbegriff des Patentanspruchs.The invention relates to a method for producing seamless pressure vessels from a CrMo steel according to the preamble of the patent claim.

Die Herstellung derartiger Druckbehälter gehört seit vielen Jahren zum bekannten Stand der Technik. Die bei der Fertigung zu beachtenden Randbedingungen sind in technischen Regelwerken wie etwa dem VdTÜV-Werkstoffblatt 431 (Fassung 03.88) niedergelegt. Außer der Zusammensetzung des zu verwendenden Werkstoffs, die teilweise mit den Gehaltsgrenzen des Patentanspruchs übereinstimmt, sind in diesem Werkstoffblatt u.a. eine Vergütungsbehandlung und ein Anlassen des fertigen Druckbehälters vorgeschrieben. Das Härten im Rahmen der Vergüting erfolgt nach einem Glühen bei 830 bis 880°C und einer Haltedauer von mindestens 1 min. je mm Wanddicke des Druckbehälters, mindestens jedoch von 15 min. mit einem anschließenden Abschrecken in öl, das maximal 50°C warm ist. Das Anlassen wird bei 530 bis 680°C mit einer Haltedauer von mindestens 2 min je mm Wanddicke, mindestens jedoch von 30 min. und mit anschließendem Abkühlen an Luft durchgeführt. Die Druckbehälter sollen mindestens die folgenden wesentlichen Werkstoffkennwerte aufweisen: 0,2 % - Dehngrenze Rp0,2 〉 755 N/mm² Zugfestigkeit Rm = 880 - 1030 N/mm² Bruchdehnung A₅ 〉 14 % Kerbschlagzähigkeit (Mittelwert von 3 Proben) aK-20°C quer 〉 25 J/cm² The production of such pressure vessels has been known for many years. The boundary conditions to be observed during production are laid down in technical regulations such as VdTÜV material sheet 431 (version 03.88). In addition to the composition of the material to be used, which partially corresponds to the content limits of the patent claim, this material specification also stipulates a tempering treatment and tempering of the finished pressure vessel. Hardening within the scope of tempering takes place after annealing at 830 to 880 ° C and a holding time of at least 1 min. per mm wall thickness of the pressure vessel, but at least 15 min. followed by quenching in oil that is a maximum of 50 ° C warm. Tempering is carried out at 530 to 680 ° C with a holding time of at least 2 min per mm wall thickness, but at least 30 min. and carried out with subsequent cooling in air. The pressure vessels should have at least the following essential material parameters: 0.2% proof stress R p0.2 〉 755 N / mm² tensile strenght R m = 880-1030 N / mm² Elongation at break A₅〉 14% Notched impact strength (average of 3 samples) a K-20 ° C across 〉 25 J / cm²

Im folgenden wird anstelle des im Stand der Technik erwähnten Meßwertes A₅ der strengare Meßwert A₂ herangezogen.In the following, instead of the measurement value A₅ mentioned in the prior art, the strict measurement value A₂ is used.

Bei einem aus dem herkömmlichen Werkstoff 34 CrMo4 mit der Analyse
   0,36 % C
   0,21 % Si
   0,68 % Mn
   0,014 % P
   0,007 % S
   1,03 % Cr
   0,24 % Mo
   0,0081 % N
hergestellten Druckbehälter mit 229 mm Durchmesser und 5,8 mm Mindestwanddicke, der nach einer 15-minütigen Glühung bei 850oC in Öl abgeschreckt, anschließend 30 min. bei 630oC angelassen und schließlich an Luft abgekühlt wurde, wurden folgende Werkstoffkenndaten gemessen: Rp0,2 = 812 N/mm² Rm = 938 N/mm² A2˝ = 15,6 % aK-20oC quer = 87 J/cm² aK-40oC quer = 52 J/cm² (mit Sprödbruchanteilen) With one made of the conventional material 34 CrMo4 with the analysis
0.36% C
0.21% Si
0.68% Mn
0.014% P
0.007% S
1.03% Cr
0.24% Mo
0.0081% N
manufactured pressure vessel with a diameter of 229 mm and a minimum wall thickness of 5.8 mm, which was quenched in oil after a 15-minute annealing at 850 o C, then 30 min. tempered at 630 o C and finally cooled in air, the following material characteristics were measured: R p0.2 = 812 N / mm² R m = 938 N / mm² A 2˝ = 15.6% a K-20 o C across = 87 J / cm² a K-40 o C across = 52 J / cm² (with brittle fraction)

Die Werte für die 0,2-Dehngrenze streuten, wobei der Streubereich 85 N/mm² betrug. Ähnliches gilt auch für die Härte, die über einen Bereich von 40 HB streute.The values for the 0.2 proof stress were scattered, the scattering range being 85 N / mm². The same applies to the hardness, which was spread over a range of 40 HB.

Für besondere Anwendungsfälle ist es erwünscht, die Festigkeitseigenschaften von Druckbehältern unter gleichzeitiger Beibehaltung der Zähigkeitseigenschaften deutlich zu steigern oder unter Beibehaltung der Festigkeitseigenschaften die Zähigkeitseigenschaften wesentlich zu verbessern.For special applications, it is desirable to significantly increase the strength properties of pressure vessels while at the same time maintaining the toughness properties, or to significantly improve the toughness properties while maintaining the strength properties.

Nach dem aus dem im Stand der Technik bekannten Herstellungsverfahren ist bei entsprechender Variation der Wärmebehandlung eine Verbesserung der Zähigkeit stets mit einer deutlichen Verringerung der Festigkeit verbunden und umgekehrt.According to the production method known from the prior art, with an appropriate variation in the heat treatment, an improvement in the toughness is always associated with a significant reduction in the strength and vice versa.

Aufgabe der Erfindung ist es, ein gattungsgemäßes Verfahren zur Herstellung von Druckbehältern aus einem CrMo-Stahl dahingehend zu verbessern, daß eine Steigerung der Festigkeitskennwerte oder Zähigkeitseigenschaften nicht mit einer entsprechenden Verschlechterung der jeweils anderen Eigenschaften verbunden ist. Außerdem sollen die mechanisch-technologischen Eigenschaften vergleichmäßigt werden.The object of the invention is to improve a generic method for producing pressure vessels from a CrMo steel in such a way that an increase in the strength values or toughness properties is not associated with a corresponding deterioration in the other properties. In addition, the mechanical-technological properties should be made more uniform.

Gelöst wird diese Aufgabe erfindungsgemäß mit den Merkmalen des Patentanspruchs 1. Vorteilhafte Weiterbildungen der Erfindung sind durch die Merkmale der Unteransprüche 2 und 3 gekennzeichnet.This object is achieved according to the invention with the features of patent claim 1. Advantageous developments of the invention are characterized by the features of subclaims 2 and 3.

Es ist bekannt, daß mit den Mikrolegierungselementen Ti und B Festigkeits- bzw. Zähigkeitseigenschaften verbessernde Wirkungen nach einem Vergüten verbunden sind. In diesem Zusammenhang ist beispielsweise auf die DE-AS 26 49 019 zu verweisen, aus der Stähle für die Herstellung von nahtlosen Stahlrohren bekannt sind, die vorzugsweise die nachfolgende Zusammensetzung aufweisen und die Härtung der Rohre aus der Walzhitze heraus ermöglichen sollen, ohne daß die Rohre sich dabei stärker verziehen: 0,05 - 0,30 % C 0,01 - 0,40 % Si 0,80 - 1,50 % Mn sowie eines oder mehrere der folgenden Elemente 0,01 - 5,00 % Cr 0,01 - 2,0 % Ni 0,01 - 1,0 % Cu 0,01 - 2,0 % Mo bis 0,10 % Al bis 0,50 % V bis 0,50 % Ti bis 0,50 % Zr bis 0,50 % Nb 0,0003 - 0,0050 % B Rest Eisen und übliche Verunreinigungen It is known that the microalloying elements Ti and B are associated with strengthening and toughening properties after tempering. In this context, reference is made, for example, to DE-AS 26 49 019, from which steels for the production of seamless steel tubes are known, which preferably have the following composition and are intended to enable the tubes to be hardened from the rolling heat without the tubes warp more: 0.05 - 0.30% C. 0.01 - 0.40% Si 0.80 - 1.50% Mn and one or more of the following 0.01 - 5.00% Cr 0.01 - 2.0% Ni 0.01 - 1.0% Cu 0.01 - 2.0% Mon up to 0.10% Al up to 0.50% V up to 0.50% Ti up to 0.50% Zr up to 0.50% Nb 0.0003 - 0.0050% B Balance iron and usual impurities

In den Ausführungsbeispielen dieser Veröffentlichung ist keine einzige Legierung angegeben, die der erfindungsgemäßen Zusammensetzung entspricht. Generell sind nämlich die dort genannten C-Gehalte zu niedrig und die Gehalte an P und S überhaupt nicht beziffert. Noch wichtiger ist es im Hinblick auf die vorliegende Erfindung, daß bei den Ti und B enthaltenden Stählen Mo überhaupt nicht und Cr in viel zu geringer Menge (0,51 %) bzw. ebenfalls überhaupt nicht vorgesehen ist. Dies entspricht vollständig der bisher üblichen Praxis, daß man CrMo-Vergütungsstähle stets unabhängig von den TiB-Vergütungsstählen gesehen hat. Über die Werte der Kerbschlagarbeit sind in der DE-AS 26 49 019 keine Angaben gemacht worden. Aus den Werten der Übergangstemperatur der Kerbschlagarbeit lassen sich darauf auch keine Rückschlüsse ziehen.In the exemplary embodiments of this publication, not a single alloy is specified which corresponds to the composition according to the invention. In general, the C contents mentioned there are too low and the P and S contents are not numbered at all. It is even more important with regard to the present invention that Mo is not provided at all in the case of the steels containing Ti and B and Cr is provided in a far too small amount (0.51%) or likewise not at all. This fully corresponds to the usual practice so far that CrMo tempered steels have always been seen independently of the TiB tempered steels. No details have been given in DE-AS 26 49 019 about the values of the impact energy. No conclusions can be drawn from the values of the transition temperature of the impact energy.

Es war daher völlig überraschend, daß bei einem Stahl mit den erfindungsgemäß eng begrenzten Legierungsanteilen bei bestimmten N-Gehalten und einem Zulegieren von Ti und B sowie bei Einhaltung der Bemessungsregel für das Ti/N-Verhältnis und Einhaltung der erfindungsgemäßen Parametergrenzen für die Wärmebehandlung derart drastische Verbesserungen hinsichtlich Festigkeit und Zähigkeit (Kerbschlagarbeit) erzielt werden können, wie sie aus den beiden in der Tabelle aufgeführten Ausführungsbeispielen zu entnehmen sind. Zur Verdeutlichung wurde darin auch das bereits angeführte Vergleichsbeispiel zum Stand der Technik aufgenommen. Alle Beispiele beziehen sich auf einen Druckbehälter mit 229 mm Durchmesser und 5,8 mm Mindestwanddicke. In den erfindungsgemäßen Ausführungsbeispielen wurde ein Werkstoff mit folgender Analyse verwendet:
   0,31 % C
   0,23 % Si
   0,72 % Mn
   0,017 % P
   0,004 % S
   0,98 % Cr
   0,21 % Mo
   0,0068 % N
   0,031 % Ti
   0,0014 % BIt was therefore completely surprising that in the case of a steel with the alloy proportions which are narrowly limited according to the invention, with certain N contents and alloying of Ti and B, as well as compliance with the dimensioning rule for the Ti / N ratio and compliance with the parameter limits according to the invention for the heat treatment, it is so drastic Improvements in strength and toughness (impact energy) can be achieved, as can be seen from the two exemplary embodiments listed in the table. For the purpose of illustration, the comparative example of the prior art already mentioned was also included. All examples relate to a pressure vessel with a diameter of 229 mm and a minimum wall thickness of 5.8 mm. A material with the following analysis was used in the exemplary embodiments according to the invention:
0.31% C
0.23% Si
0.72% Mn
0.017% P
0.004% S
0.98% Cr
0.21% Mo
0.0068% N
0.031% Ti
0.0014% B

Im erfindungsgemäßen Beispiel 1 wurde bei geringfügig verbessertem Rp0,2-Wert von 819 N/mm² eine Steigerung der Kerbschlagzähigkeit bei -20oC um 55 % und bei -40oC sogar um 108 % erreicht. Bemerkenswert ist, daß sich die Breite des Streubandes der Dehngrenze Rp0,2 um etwa 44 % und die Härte um 35 % gegenüber den Vergleichswerten gemäß dem Stand der Technik verringerten.In Inventive Example 1 was slightly improved when R p0.2 value of 819 N / mm², an increase of the notched impact strength at -20 ° C by 55% and even reaching at -40 o C to 108%. It is noteworthy that the width of the scattering band of the proof stress R p0.2 decreased by about 44% and the hardness by 35% compared to the comparative values according to the prior art.

Das Beispiel 2 zielte auf eine Steigerung der Festigkeit unter weitgehender Beibehaltung der Zähigkeitseigenschaften ab. Mit Werten für die Kerbschlagzähigkeit von 95 J/cm² und 68 J/cm² bei -20oC bzw. -40oC ergaben sich sogar noch Zähigkeitsverbesserungen gegenüber dem Vergleichsbeispiel um etwa 9 % bzw. 31 %; die Dehnung A2˝ lag dabei mit 13,5 % nur geringfügig unter dem an sich geforderten Mindestwert von 14 %. Diese Beeinträchtigung ist jedoch vor dem Hintergrund, daß die Dehngrenze Rp0,2 ohne Zähigkeitseinbuße von 812 N/mm² auf 1025 N/mm², also um etwa 26 % gesteigert werden konnte, ohne weiteres tolerierbar. Die Breite der Streubänder der Dehngrenze und der Härte verringerten sich dabei gleichzeitig noch um 39 % bzw. 22 %.Example 2 aimed to increase the strength while largely maintaining the toughness properties. With values for the notched impact strength of 95 J / cm² and 68 J / cm² at -20 o C and -40 o C there were even improvements in toughness compared to the comparative example by about 9% and 31%; The elongation A 2˝ was 13.5%, only slightly below the minimum value of 14% required per se . However, this impairment is easily tolerable against the background that the yield strength R p0.2 could be increased from 812 N / mm² to 1025 N / mm², ie by about 26%, without sacrificing toughness. The spread of the yield strength and the hardness were reduced by 39% and 22%, respectively.

Die beiden Ausführungsbeispiele der Erfindung machen deutlich, daß mit geringem Aufwand erhebliche Verbesserungen der Festigkeits- und/oder der Zähigkeitseigenschaften an nahtlosen Druckbehältern aus CrMo-Stahl erreicht werden können. Tabelle Kenndaten Vergleichsbeispiel Erfindung Beispiel 1 Beispiel 2 Austenitisierung Temperatur (oC) 850 850 830 Haltezeit (min) 15 15 15 Abschrecken Öl Öl Öl Anlassen Temperatur (oC) 630 630 530 Haltezeit (min) 30 30 30 Rp0,2 (N/mm²) 812 819 1025 Δ Rp0,2 (N/mm²) 85 48 52 Rm (N/mm²) 938 962 1110 A2˝ (%) 15,6 16,1 13,5 aK-20°C quer (J/cm²) 87 135 95 aK-40°C quer (J/cm²) 52 (mit Sprödbruchanteilen) 108 (ohne Sprödbruchanteile) 68 (mit Sprödbruchanteilen) Δ Härte (HB) 40 26 31 The two exemplary embodiments of the invention make it clear that considerable improvements in strength and / or toughness properties can be achieved on seamless pressure vessels made of CrMo steel with little effort. table Characteristics Comparative example invention example 1 Example 2 Austenitization Temperature ( o C) 850 850 830 Holding time (min) 15 15 15 Scare off oil oil oil Start Temperature ( o C) 630 630 530 Holding time (min) 30th 30th 30th R p0.2 (N / mm²) 812 819 1025 Δ R p0.2 (N / mm²) 85 48 52 R m (N / mm²) 938 962 1110 A 2˝ (%) 15.6 16.1 13.5 a K-20 ° C across (J / cm²) 87 135 95 a K-40 ° C across (J / cm²) 52 (with brittle fraction) 108 (without brittle fraction) 68 (with brittle fraction) Δ hardness (HB) 40 26 31

Claims (3)

  1. A process for the manufacture of seamless pressure vessels by hot deforming of steel tubes of a CrMo steel, killed with aluminium, with (% by weight)
       0.28 - 0.38 % C
       0.15 - 0.40 % Si
       0.45 - 0.90 % Mn
       max. 0.02 % P
       max. 0.005 % S
       0.90 - 1.30 % Cr
       0.15 - 0.35 % Mo
       remainder iron and usual impurities,
    which with a given N content of 0.003 - 0.010 % additionally contains
    0.010 - 0.0140 % Ti and
       0.001 - 0.003 % B
    in which the Ti/N ratio amounts to at least 3.4, in which the pressure vessels are tempered after hot deformation, by being austenitised at 830 - 880 °C, then cooled to ambient temperature at a cooling rate of 5 - 15 K/s, thereafter tempered at temperatures - depending on the desired degree of strength - between 510 °C and 660 °C and finally cooled in air.
  2. A process according to Claim 1,
    characterised in that
    to increase the impact toughness, the tempering is carried out at 620 - 660 °C.
  3. A process according to Claim 1,
    characterised in that
    to increase the strength, the tempering is carried out at 510 - 550 °C.
EP89250061A 1988-11-01 1989-10-23 Process for manufacturing seamless pressure vessels Expired - Lifetime EP0367360B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3837400A DE3837400C2 (en) 1988-11-01 1988-11-01 Process for the production of seamless pressure vessels
DE3837400 1988-11-01

Publications (3)

Publication Number Publication Date
EP0367360A2 EP0367360A2 (en) 1990-05-09
EP0367360A3 EP0367360A3 (en) 1991-09-11
EP0367360B1 true EP0367360B1 (en) 1994-08-03

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US (1) US5030297A (en)
EP (1) EP0367360B1 (en)
AT (1) ATE109515T1 (en)
DE (2) DE3837400C2 (en)
ES (1) ES2057097T3 (en)

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US6488790B1 (en) 2001-01-22 2002-12-03 International Steel Group Inc. Method of making a high-strength low-alloy hot rolled steel
CN104498830B (en) * 2014-12-30 2017-06-23 南阳汉冶特钢有限公司 A kind of structural alloy steel and its production method
WO2020250009A1 (en) * 2019-06-12 2020-12-17 Arcelormittal A cold rolled martensitic steel and a method of martensitic steel thereof
CN113862556B (en) * 2021-08-05 2022-08-05 邯郸新兴特种管材有限公司 4140 medium-thick-wall seamless steel pipe and production method thereof

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Publication number Publication date
DE3837400C2 (en) 1995-02-23
ES2057097T3 (en) 1994-10-16
EP0367360A2 (en) 1990-05-09
DE58908140D1 (en) 1994-09-08
US5030297A (en) 1991-07-09
ATE109515T1 (en) 1994-08-15
DE3837400A1 (en) 1990-05-03
EP0367360A3 (en) 1991-09-11

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