EP0308361B1 - Process for manufacturing steel pressure vessels - Google Patents
Process for manufacturing steel pressure vessels Download PDFInfo
- Publication number
- EP0308361B1 EP0308361B1 EP88730190A EP88730190A EP0308361B1 EP 0308361 B1 EP0308361 B1 EP 0308361B1 EP 88730190 A EP88730190 A EP 88730190A EP 88730190 A EP88730190 A EP 88730190A EP 0308361 B1 EP0308361 B1 EP 0308361B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- pressure vessels
- steel
- titanium
- steel pressure
- manufacturing steel
- 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 - Lifetime
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 19
- 239000010959 steel Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 239000010955 niobium Substances 0.000 claims abstract description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract 6
- 229910052742 iron Inorganic materials 0.000 claims abstract 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000005864 Sulphur Substances 0.000 claims abstract 2
- 239000012535 impurity Substances 0.000 claims abstract 2
- 239000011572 manganese Substances 0.000 claims abstract 2
- 239000011733 molybdenum Substances 0.000 claims abstract 2
- 239000011574 phosphorus Substances 0.000 claims abstract 2
- 239000010703 silicon Substances 0.000 claims abstract 2
- 238000005496 tempering Methods 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- 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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- 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
- C21D1/18—Hardening; Quenching with or without subsequent tempering
-
- 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
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
Definitions
- the invention relates to a method for producing pressure vessels made of steel according to the preamble of patent claim 1.
- tempered steels such as material 34 CrMo4 are generally used in pressure vessel construction.
- the object of the invention is therefore to provide a method with which pressure vessels can be produced which do not have these disadvantages.
- a reduction in the pressure vessel weight should be made possible by increased strength properties (reduction in wall thicknesses) with sufficient safety and at low costs, the material used having good welding properties and at least the following strength and toughness parameters transverse to the direction of deformation: 0.2% - proof stress over 900 N / mm2 Proof stress ratio maximum 95% Constriction at least 16% ISO V impact energy at +20 ° C over 80 J ISO V impact energy at -60 ° C over 36 J
- This object is achieved by a method with the characterizing features of claim 1.
- chromium is advantageously added to the steel used in accordance with claim 2 to a maximum of 0.3%.
- the heat-treatable steel used according to the invention can be welded without problems, that is to say free of hot cracks, by the usual methods.
- it can be oil and water tempered.
- extraordinarily good strength and toughness values result. Some of these clearly exceed the set limit values.
- a titanium / nitrogen ratio of 3.6 to 6.5 is required to maximize the strengthening effect of boron.
- niobium can further increase the fine-grained nature and thus the toughness of the steel according to the invention
- the proof stress ratio can increase to approximately 95% in the steel according to the invention, there is nevertheless sufficient security against disassembly of the container, because the constriction of the fracture can in any case be kept at a value of at least 16%. It is particularly important that the impact energy at -60 ° C transversely to the direction of deformation (ISO-V impact tests) is over 36 J. This also makes the material suitable for use at low temperatures, such as those found under arctic conditions.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Heat Treatment Of Articles (AREA)
- Treatment Of Steel In Its Molten State (AREA)
- Pressure Vessels And Lids Thereof (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von Druckbehältern aus Stahl gemäß dem Oberbegriff des Patentanspruchs 1.The invention relates to a method for producing pressure vessels made of steel according to the preamble of patent claim 1.
Die Sicherheitsanforderungen an Druckbehälter, wie sie beispielsweise in den "Technische Regeln Druckgase" des Deutschen Druckbehälterausschusses (DBA) festgelegt sind, schlagen sich in gleichermaßen hohen Anforderungen an die eingesetzten Werkstoffe nieder. Bei Stahlflaschen (Prüfdruck 300 bar) wird in diesem Zusammenhang gefordert:
0,2% - Dehngrenze über 755 N/mm²
Zugfestigkeit 880 - 1030 N/mm²
ISO-V-Kerbschlagarbeit (quer) bei -20°C über 25 J Dehngrenzenverhältnis unter 90%.The safety requirements for pressure vessels, such as those specified in the "Technical Rules for Compressed Gases" of the German Pressure Vessel Committee (DBA), are reflected in equally high requirements for the materials used. For steel bottles (test pressure 300 bar) the following is required:
0.2% proof stress over 755 N / mm²
Tensile strength 880 - 1030 N / mm²
ISO-V impact energy (crosswise) at -20 ° C over 25 J proof stress ratio under 90%.
Zur Einhaltung dieser Forderungen werden im Druckbehälterbau im allgemeinen Vergütungsstähle wie beispielsweise Werkstoff 34 CrMo4 eingesetzt.To meet these requirements, tempered steels such as material 34 CrMo4 are generally used in pressure vessel construction.
Um den Transport und die Handhabung von Druckbehältern zu verbilligen bzw. zu erleichtern, ist man bestrebt, den Druckbehälter möglichst gewichtsarm, d.h. mit geringen Wanddicken, herzustellen. Dabei sollen die Sicherheitsanforderungen jedoch voll erfüllt bleiben. Dies ist aber nur möglich, wenn die Festigkeitseigenschaften des verwendeten Werkstoffs entsprechend gesteigert werden. Das aber ist bei den üblichen Vergütungsstählen unter Einhaltung der genannten Bedingungen nur in geringem Maße durchführbar.In order to make the transportation and handling of pressure vessels cheaper or easier, efforts are being made to manufacture the pressure vessel as light as possible, ie with small wall thicknesses. However, the security requirements should remain fully met. However, this is only possible if the strength properties of the used Material are increased accordingly. However, this is only feasible to a small extent with the conventional tempering steels, provided the conditions mentioned are met.
Ein weiterer Nachteil ist in der eingeschränkten Schweißbarkeit dieser Stähle zu sehen, die durch den hohen Kohlenstoff-Gehalt von über 0,3% bedingt ist. Daneben entspricht auch die in der Regel erforderliche Ölvergütung für solche Stähle nicht mehr den heutigen Anforderungen an moderne Fertigungsanlagen, die nach Möglichkeit eine Wasservergütung vorsehen. Schließlich weisen die für die Behälterfertigung üblicherweise verwendeten Werkstoffe Mängel hinsichtlich ihrer Kerbschlagzähigkeit bei tiefen Temperaturen auf. Einsatztemperaturen von unter -20 °C sind schon als problematisch anzusehen.Another disadvantage is the limited weldability of these steels, which is due to the high carbon content of over 0.3%. In addition, the generally required oil remuneration for such steels no longer meets today's requirements for modern production facilities, which provide for water remediation where possible. Finally, the materials commonly used for container production have shortcomings in their impact strength at low temperatures. Operating temperatures of below -20 ° C are problematic.
Aufgabe der Erfindung ist es daher, ein Verfahren anzugeben, mit dem Druckbehälter herstellbar sind, die diese Nachteile nicht aufweisen. Insbesondere soll eine Verringerung des Druckbehältergewichts durch erhöhte Festigkeitseigenschaften (Reduzierung der Wanddicken) bei ausreichender Sicherheit und unter günstigen Kosten ermöglicht werden, wobei der verwendete Werkstoff gute Schweißeigenschaften und mindestens folgende Festigkeits- und Zähigkeitskennwerte quer zur Verformungsrichtung aufweisen soll:
0,2% - Dehngrenze über 900 N/mm²
Dehngrenzenverhältnis maximal 95%
Brucheinschnürung mindestens 16%
ISO-V-Kerbschlagarbeit bei +20 °C über 80 J
ISO-V-Kerbschlagarbeit bei -60 °C über 36 J
Gelöst wird diese Aufgabe durch ein Verfahren mit den kennzeichnenden Merkmalen des Patentanspruchs 1. Zur weiteren Verbesserung der Durchhärtbarkeit der Druckbehälter (insbesondere bei Wanddicken über 30 mm) wird dem verwendeten Stahl vorteilhaft entsprechend Patentanspruch 2 Chrom bis maximal 0,3% zugesetzt.The object of the invention is therefore to provide a method with which pressure vessels can be produced which do not have these disadvantages. In particular, a reduction in the pressure vessel weight should be made possible by increased strength properties (reduction in wall thicknesses) with sufficient safety and at low costs, the material used having good welding properties and at least the following strength and toughness parameters transverse to the direction of deformation:
0.2% - proof stress over 900 N / mm²
Proof stress ratio maximum 95%
Constriction at least 16%
ISO V impact energy at +20 ° C over 80 J
ISO V impact energy at -60 ° C over 36 J
This object is achieved by a method with the characterizing features of claim 1. To further improve the hardenability of the pressure vessels (in particular for wall thicknesses above 30 mm), chromium is advantageously added to the steel used in accordance with claim 2 to a maximum of 0.3%.
Der erfindungsgemäß verwendete Vergütungsstahl ist trotz des relativ hohen Kohlenstoffanteils von bis zu 0,25% in der vorgegebenen Legierungszusammensetzung nach den üblichen Verfahren problemlos, d.h. heißrißfrei schweißbar. Darüberhinaus kann er sowohl öl- als auch wasservergütet werden. In Kombination mit der Mischkristallverfestigung und der Verbesserung der Durchhärtbarkeit durch Bor ergeben sich außerordentlich gute Festigkeits- und Zähigkeitskennwerte. Diese überschreiten die gesetzten Grenzwerte zum Teil deutlich. Um die festigkeitssteigernde Wirkung des Bors maximal ausnutzen zu können, ist ein Titan/Stickstoff-Verhältnis von 3,6 bis 6,5 erforderlich. Durch Zusatz von bis zu 0,04% Niob kann die Feinkörnigkeit und damit die Zähigkeit des erfindungsgemäßen Stahls noch weiter gesteigert werden.Wenngleich sich das Dehngrenzenverhältnis bei dem erfindungsgemäßen Stahl auf etwa 95% erhöhen kann, so ist dennoch eine ausreichende Sicherheit gegen ein Zerlegen des Behälters vorhanden, weil die Brucheinschnürung auf jeden Fall auf Werten von mindestens 16% gehalten werden kann. Besonders wesentlich ist, daß die Kerbschlagarbeit bei -60 °C quer zur Verformungsrichtung (ISO-V-Kerbschlagproben) über 36 J liegt. Dies macht den Werkstoff auch für eine Anwendung bei tiefen Temperaturen, wie sie unter arktischen Bedingungen herrschen, verwendbar.Despite the relatively high carbon content of up to 0.25% in the specified alloy composition, the heat-treatable steel used according to the invention can be welded without problems, that is to say free of hot cracks, by the usual methods. In addition, it can be oil and water tempered. In combination with the solid solution strengthening and the improvement of the hardenability by boron, extraordinarily good strength and toughness values result. Some of these clearly exceed the set limit values. A titanium / nitrogen ratio of 3.6 to 6.5 is required to maximize the strengthening effect of boron. The addition of up to 0.04% niobium can further increase the fine-grained nature and thus the toughness of the steel according to the invention Although the proof stress ratio can increase to approximately 95% in the steel according to the invention, there is nevertheless sufficient security against disassembly of the container, because the constriction of the fracture can in any case be kept at a value of at least 16%. It is particularly important that the impact energy at -60 ° C transversely to the direction of deformation (ISO-V impact tests) is over 36 J. This also makes the material suitable for use at low temperatures, such as those found under arctic conditions.
Die besondere Eignung des erfindungsgemäßen Stahl für den Bau von Druckbehältern wird durch die beiden nachfolgenden Beispiele weiter verdeutlicht.The particular suitability of the steel according to the invention for the construction of pressure vessels is further illustrated by the two examples below.
Für eine Flasche (Wanddicke 4 mm) aus einem Stahl mit der Zusammensetzung:
0,24 % C
1,4 % Mn
0,28 % Si
0,013 % P
0,0018 % S
0,29 % Mo
0,023 % Ti
0,0020 % B
0,0037 % N
ergaben sich nach der erfindungsgemäßen Vergütungsbehandlung (15 min bei 870 °C, Abschrecken im Ölbad; 30 min bei 600 °C, Abkühlen an Luft) folgende Eigenschaften:
0,2 % - Dehngrenze 903 N/mm²
Zugfestigkeit 950 N/mm²
Dehngrenzenverhältnis 95%
Brucheinschnürung 20%
ISO-V-Kerbschlagarbeit bei +20 °C (quer) 133 J
ISO-V-Kerbschlagarbeit bei -60 °C (quer) 58 J.For a bottle (wall thickness 4 mm) made of steel with the composition:
0.24% C
1.4% Mn
0.28% Si
0.013% P
0.0018% S
0.29% Mo
0.023% Ti
0.0020% B
0.0037% N
After the heat treatment according to the invention (15 min at 870 ° C, quenching in an oil bath; 30 min at 600 ° C, cooling in air), the following properties resulted:
0.2% - yield strength 903 N / mm²
Tensile strength 950 N / mm²
Proof ratio 95%
Constriction 20%
ISO-V impact energy at +20 ° C (transverse) 133 J
ISO-V impact energy at -60 ° C (transverse) 58 J.
Für einen Serienbehälter (6 mm Wanddicke) aus einem Stahl mit der Zusammensetzung:
0,2 % C
1,74 % Mn
0,3 % Si
0,013 % P
0,0014 % S
0,30 % Mo
0,021 % Ti
0,0022 % B
0,0048 % N
ergaben sich nach der erfindungsgemäßen Vergütungsbehandlung (15 Min bei 880 °C, Abschrecken im Wasserbad; 30 min bei 500 °C, Abkühlen an Luft) folgende Eigenschaften:
0,2 % - Dehngrenze 992 N/mm²
Zugfestigkeit 1042 N/mm²
Dehngrenzenverhältnis 95%
Brucheinschnürung 17%
ISO-V-Kerbschlagarbeit bei +20 °C (quer) 114 J
ISO-V-Kerbschlagarbeit bei -60 °C (quer) 40 J.For a series container (6 mm wall thickness) made of steel with the composition:
0.2% C
1.74% Mn
0.3% Si
0.013% P
0.0014% S
0.30% Mo
0.021% Ti
0.0022% B
0.0048% N
After the heat treatment according to the invention (15 minutes at 880 ° C., quenching in a water bath; 30 minutes at 500 ° C., cooling in air), the following properties resulted:
0.2% proof stress 992 N / mm²
Tensile strength 1042 N / mm²
Proof ratio 95%
Fracture reduction 17%
ISO-V impact energy at +20 ° C (transverse) 114 J
ISO-V impact energy at -60 ° C (transverse) 40 J.
Claims (2)
- A method for producing steel pressure vessels by hot and/or cold shaping and subsequent hardening and tempering, characterised in that a steel having the composition
0.15 - 0.26 % carbon 1.25 - 2.00 % manganese 0.2 - 0.5 % silicon at most 0.02 % phosphorus at most 0.005 % sulphur 0.1 - 0.5 % molybdenum 0.010 - 0.035 % titanium 0.0030 - 0.0100 % N 0.001 - 0.003 % boron 0 - 0.04 % niobium remainder iron and usual impurities - A method according to Claim 1, characterised in that the steel used additionally contains at most 0.3% chromium at the expense of the residual element iron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT88730190T ATE95844T1 (en) | 1987-09-16 | 1988-08-23 | PROCESS FOR MANUFACTURING STEEL PRESSURE TANKS. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19873731481 DE3731481A1 (en) | 1987-09-16 | 1987-09-16 | METHOD FOR THE PRODUCTION OF STEEL PRESSURE TANKS |
| DE3731481 | 1987-09-16 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0308361A1 EP0308361A1 (en) | 1989-03-22 |
| EP0308361B1 true EP0308361B1 (en) | 1993-10-13 |
Family
ID=6336365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP88730190A Expired - Lifetime EP0308361B1 (en) | 1987-09-16 | 1988-08-23 | Process for manufacturing steel pressure vessels |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0308361B1 (en) |
| AT (1) | ATE95844T1 (en) |
| DE (2) | DE3731481A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1013099C2 (en) * | 1999-09-20 | 2001-03-21 | Matthijs De Jong | Pressurized tank for liquefied gas, especially for gas tankers, comprises a steel material with specific silicon, chromium, copper, molybdenum and nickel contents |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD79594A (en) * | ||||
| US3328211A (en) * | 1963-12-05 | 1967-06-27 | Ishikawajima Harima Heavy Ind | Method of manufacturing weldable, tough and high strength steel for structure members usable in the ashot-state and steel so made |
| FR2287519A1 (en) * | 1974-10-07 | 1976-05-07 | Kobe Steel Ltd | Weldable structural steel - which is resistant to embrittlement in the heat affected zone |
| JPS52152814A (en) * | 1976-06-14 | 1977-12-19 | Nippon Steel Corp | Thermo-mechanical treatment of seamless steel pipe |
| JPS62196326A (en) * | 1986-02-24 | 1987-08-29 | Sumitomo Metal Ind Ltd | Manufacture of high-strength steel excellent in surface toughness |
-
1987
- 1987-09-16 DE DE19873731481 patent/DE3731481A1/en not_active Withdrawn
-
1988
- 1988-08-23 EP EP88730190A patent/EP0308361B1/en not_active Expired - Lifetime
- 1988-08-23 DE DE88730190T patent/DE3884900D1/en not_active Expired - Fee Related
- 1988-08-23 AT AT88730190T patent/ATE95844T1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| ATE95844T1 (en) | 1993-10-15 |
| EP0308361A1 (en) | 1989-03-22 |
| DE3884900D1 (en) | 1993-11-18 |
| DE3731481A1 (en) | 1989-04-06 |
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