EP0297035A1 - Aluminium alloy for superplastic deformation - Google Patents

Aluminium alloy for superplastic deformation Download PDF

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Publication number
EP0297035A1
EP0297035A1 EP88810378A EP88810378A EP0297035A1 EP 0297035 A1 EP0297035 A1 EP 0297035A1 EP 88810378 A EP88810378 A EP 88810378A EP 88810378 A EP88810378 A EP 88810378A EP 0297035 A1 EP0297035 A1 EP 0297035A1
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EP
European Patent Office
Prior art keywords
max
aluminum alloy
alloy according
iron
manganese
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.)
Granted
Application number
EP88810378A
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German (de)
French (fr)
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EP0297035B1 (en
Inventor
Heinrich Homberger
Jürgen Timm
Pedro Rodrigues
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.)
3A Composites International AG
Original Assignee
Alusuisse Holdings AG
Schweizerische Aluminium AG
Alusuisse Lonza Services Ltd
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Publication date
Application filed by Alusuisse Holdings AG, Schweizerische Aluminium AG, Alusuisse Lonza Services Ltd filed Critical Alusuisse Holdings AG
Priority to AT88810378T priority Critical patent/ATE70566T1/en
Publication of EP0297035A1 publication Critical patent/EP0297035A1/en
Application granted granted Critical
Publication of EP0297035B1 publication Critical patent/EP0297035B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S420/00—Alloys or metallic compositions
    • Y10S420/902—Superplastic

Definitions

  • the invention relates to an aluminum alloy as a material for superplastic forming.
  • Superplastically formable materials have been known for a long time. The most important requirement here is the fine-grained nature of the material to be formed. For example, a sheet size of less than 10 ⁇ m is required for sheets that are to be superplastically formed. The grains are also said to be almost globulitic. In addition, no significant coarsening of the grains may occur during the superplastic forming, which is carried out at about 500 ° C. In the case of the known alloys suitable for superplastic forming, these requirements generally require complex thermomechanical pretreatment.
  • the inventor has set the goal of providing an aluminum alloy suitable as a material for superplastic forming, which can be processed into superplastic formable sheets without special thermomechanical pretreatment.
  • the solution to the problem is that the alloy 0.8 - 2.5% iron, 3.5 - 6.0% magnesium, 0.1 - 0.6% manganese, 0.05 - 0.5% zircon, Max. 6.0% zinc, Max. 3.0% copper, Max. 0.3% silicon, Max. 0.05% titanium, Max. 0.05% chromium, as well as the rest contains aluminum of commercial purity.
  • the maximum permissible iron content of 2.5% is provided when the alloy is processed using casting rolls or when using other casting processes with abrupt solidification. If the alloy is cast using conventional or electromagnetic continuous casting molds, the maximum permissible iron content is 1.6%. If these upper limits for iron are adhered to, undesired solidification can be prevented. In general, however, it should be noted that the addition of manganese should be kept low if the iron content is high.
  • the addition of zinc and / or copper serves to generally increase the strength of the alloy.
  • the zinc addition is preferably between 3.0 and 4.0%.
  • An alloy that is particularly suitable as a material for superplastic forming has the following composition: 1.1 - 1.3% iron, 4.3 - 4.7% magnesium, 0.1 - 0.3% manganese, 0.1 - 0.2% zircon, Max. 0.15% silicon, Max. 0.05% titanium, Max. 0.05% chromium, The rest of aluminum is commercially available.
  • alloy composition refers to percentages by weight.
  • the alloy according to the invention is preferably cast into rolled bars by means of conventional or electromagnetic continuous casting molds and can be processed into superplastic formable sheets without special thermomechanical pretreatment.
  • the degree of deformation during cold rolling should be at least 60%, preferably at least 70%. If intermediate annealing is switched on, the minimum degree of deformation refers to cold rolling to the final thickness after intermediate annealing.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Powder Metallurgy (AREA)
  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Forging (AREA)

Abstract

An aluminium alloy suitable as a material for superplastic forming contains 0.8-2.5% or iron, 3.5-6.0% of magnesium, 0.1-0.6% of manganese, 0.05-0.5% of zirconium, at most 6.0% of zinc, at most 3.0% of copper, at most 0.3% of silicon, at most 0.05% of titanium and at most 0.05% of chromium, the remainder being aluminium of commercial purity. The alloy can be processed to give superplastically formable sheets without separate thermomechanical pretreatment.

Description

Die Erfindung betrifft eine Aluminiumlegierung als Werk­stoff für superplastische Umformung.The invention relates to an aluminum alloy as a material for superplastic forming.

Superplastisch umformbare Werkstoffe sind seit langem be­kannt. Wesentlichste Voraussetzung ist hierbei die Feinkör­nigkeit des umzuformenden Werkstoffs. So benötigt man etwa bei Blechen, welche superplastisch umgeformt werden sollen, eine Korngrösse von bevorzugt weniger als 10 µm. Die Körner sollen zudem nahezu globulitisch vorliegen. Ueberdies darf sich während der superplastischen Umformung, welche bei et­wa 500°C durchgeführt wird, auch keine wesentliche Vergrö­berung der Körner einstellen. Diese Anforderungen machen bei den bekannten, für die superplastische Umformung geeig­neten Legierungen im allgemeinen eine aufwendige thermome­chanische Vorbehandlung erforderlich.Superplastically formable materials have been known for a long time. The most important requirement here is the fine-grained nature of the material to be formed. For example, a sheet size of less than 10 µm is required for sheets that are to be superplastically formed. The grains are also said to be almost globulitic. In addition, no significant coarsening of the grains may occur during the superplastic forming, which is carried out at about 500 ° C. In the case of the known alloys suitable for superplastic forming, these requirements generally require complex thermomechanical pretreatment.

Angesichts dieser Gegebenheiten hat sich der Erfinder das Ziel gesetzt, eine als Werkstoff für superplastische Umfor­mung geeignete Aluminiumlegierung bereitzustellen, die ohne besondere thermomechanische Vorbehandlung zu superplastisch umformbaren Blechen verarbeitet werden kann.In view of these circumstances, the inventor has set the goal of providing an aluminum alloy suitable as a material for superplastic forming, which can be processed into superplastic formable sheets without special thermomechanical pretreatment.

Zur Lösung der gestellten Aufgabe führt, dass die Legierung
0,8 - 2,5 % Eisen,
3,5 - 6,0 % Magnesium,
0,1 - 0,6 % Mangan,
0,05 - 0,5 % Zirkon,
max. 6,0 % Zink,
max. 3,0 % Kupfer,
max. 0,3 % Silicium,
max. 0,05 % Titan,
max. 0,05 % Chrom,
sowie als Rest Aluminium handelsüblicher Reinheit enthält.The solution to the problem is that the alloy
0.8 - 2.5% iron,
3.5 - 6.0% magnesium,
0.1 - 0.6% manganese,
0.05 - 0.5% zircon,
Max. 6.0% zinc,
Max. 3.0% copper,
Max. 0.3% silicon,
Max. 0.05% titanium,
Max. 0.05% chromium,
as well as the rest contains aluminum of commercial purity.

Der maximal zulässige Eisengehalt von 2,5 % ist bei Verar­beitung der Legierung über Giesswalzen oder bei Anwendung anderer Giessverfahren mit schroffer Erstarrung vorgesehen. Wird die Legierung mittels konventioneller oder elektromag­netischer Stranggiesskokillen vergossen, so liegt der maxi­mal zulässige Eisengehalt bei 1,6 %. Bei Einhaltung dieser oberen Gehaltsgrenzen für Eisen können unerwünschte Vorer­starrungen verhindert werden. Generell ist jedoch zu beach­ten, dass bei hohem Eisengehalt der Zusatz an Mangan eher gering gehalten werden sollte.The maximum permissible iron content of 2.5% is provided when the alloy is processed using casting rolls or when using other casting processes with abrupt solidification. If the alloy is cast using conventional or electromagnetic continuous casting molds, the maximum permissible iron content is 1.6%. If these upper limits for iron are adhered to, undesired solidification can be prevented. In general, however, it should be noted that the addition of manganese should be kept low if the iron content is high.

Für die einzelnen Elemente haben sich die nachfolgenden Ge­haltsbereiche als bevorzugt herausgestellt:
1,0 - 1,4 % Eisen,
4,0 - 5,0 % Magnesium,
0,1 - 0,3 % Mangan,
0,1 - 0,2 % Zirkon,
max. 0,15 % Silicium.The following salary ranges have been found to be preferred for the individual elements:
1.0 - 1.4% iron,
4.0 - 5.0% magnesium,
0.1 - 0.3% manganese,
0.1 - 0.2% zircon,
Max. 0.15% silicon.

Ein Zusatz von Zink und/oder Kupfer dient zur generellen Festigkeitssteigerung der Legierung. Hierbei liegt der Zinkzusatz bevorzugt zwischen 3,0 und 4,0 %.The addition of zinc and / or copper serves to generally increase the strength of the alloy. The zinc addition is preferably between 3.0 and 4.0%.

Eine als Werkstoff für superplastische Umformung besonders geeignete Legierung weist die folgende Zusammensetzung auf:
1,1 - 1,3 % Eisen,
4,3 - 4,7 % Magnesium,
0,1 - 0,3 % Mangan,
0,1 - 0,2 % Zirkon,
max. 0,15 % Silicium,
max. 0,05 % Titan,
max. 0,05 % Chrom,
Rest Aluminium handelsüblicher Reinheit.An alloy that is particularly suitable as a material for superplastic forming has the following composition:
1.1 - 1.3% iron,
4.3 - 4.7% magnesium,
0.1 - 0.3% manganese,
0.1 - 0.2% zircon,
Max. 0.15% silicon,
Max. 0.05% titanium,
Max. 0.05% chromium,
The rest of aluminum is commercially available.

Alle Gehaltsangaben betreffend die Legierungszusammenset­zung beziehen sich auf Gewichts-Prozente.All content information regarding the alloy composition refer to percentages by weight.

Die erfindungsgemässe Legierung wird bevorzugt mittels kon­ventioneller oder elektromagnetischer Stranggiesskokillen zu Walzbarren vergossen und lässt sich ohne besondere ther­momechanische Vorbehandlung zu superplastisch umformbaren Blechen verarbeiten. Damit die geforderte Feinkörnigkeit erreicht wird, soll der Verformungsgrad beim Kaltwalzen mindestens 60 %, vorzugsweise mindestens 70 %, betragen. Wird eine Zwischenglühung eingeschaltet, so bezieht sich der Mindestverformungsgrad auf das Kaltwalzen auf Enddicke nach erfolgter Zwischenglühung.The alloy according to the invention is preferably cast into rolled bars by means of conventional or electromagnetic continuous casting molds and can be processed into superplastic formable sheets without special thermomechanical pretreatment. In order to achieve the required fine grain size, the degree of deformation during cold rolling should be at least 60%, preferably at least 70%. If intermediate annealing is switched on, the minimum degree of deformation refers to cold rolling to the final thickness after intermediate annealing.

Die Vorteilhaftigkeit der erfindungsgemässen Legierung wird nachstehend anhand eines Ausführungsbeispieles gezeigt.The advantageousness of the alloy according to the invention is shown below using an exemplary embodiment.

Beispielexample

Eine Legierung mit 1,2 % Eisen, 4,54 % Magnesium, 0,24 % Mangan, 0,15 % Zirkon, 0,10 % Silicium, sowie 0,03 % Titan wurde mittels einer Stranggiesskokille zu einem Walzbarren von 70 mm Dicke vergossen und während 24 Stunden bei einer Temperatur von 450°C homogenisiert. Der Barren wurde an­schliessend auf 500°C angewärmt und zu einer Dicke von 12 mm warmgewalzt. Nach dem Abkühlen wurden die Warmwalz­platten wie folgt kaltgewalzt:
Variante A: Ohne Zwischenglühung kaltgewalzt auf 3 mm;
Variante B: Kaltgewalzt auf 6 mm, 12 Std. bei 400°C zwi­schengeglüht, kaltgewalzt auf 1,2 mm.
Zur Prüfung des superplastischen Umformverhaltens wurden aus den kaltgewalzten Blechen Zugproben mit einer Schaft­breite von 10 mm und einer Messlänge von 20 mm gefertigt und auf einer Zugmaschine bei einer Temperatur von 490°C mit einer wahren Dehngeschwindigkeit von 5 x 10⁻⁴ s⁻¹ bis zum Bruch verformt. Die erreichten Dehnungswerte betrugen für die Variante A 550 %, für die Variante B 585 %.An alloy with 1.2% iron, 4.54% magnesium, 0.24% manganese, 0.15% zircon, 0.10% silicon, and 0.03% titanium was made into a roll ingot 70 mm thick using a continuous casting mold poured and homogenized for 24 hours at a temperature of 450 ° C. The ingot was then heated to 500 ° C and hot rolled to a thickness of 12 mm. After cooling, the hot rolled plates were cold rolled as follows:
Variant A: Cold rolled to 3 mm without intermediate annealing;
Variant B: Cold rolled to 6 mm, annealed for 12 hours at 400 ° C, cold rolled to 1.2 mm.
To test the superplastic forming behavior, tensile specimens with a shank width of 10 mm and a measuring length of 20 mm were produced from the cold-rolled sheets and on a tractor at a temperature of 490 ° C with a true expansion speed of 5 x 10⁻⁴ s⁻¹ up to Fracture deformed. The elongation values achieved were 550% for variant A and 585% for variant B.

Claims (9)

1. Aluminiumlegierung als Werkstoff für superplastische Um­formung, dadurch gekennzeichnet, dass die Legierung
0,8 - 2,5 % Eisen,
3,5 - 6,0 % Magnesium,
0,1 - 0,6 % Mangan,
0,05 - 0,5 % Zirkon,
max. 6,0 % Zink,
max. 3,0 % Kupfer,
max. 0,3 % Silicium,
max. 0,05 % Titan,
max. 0,05 % Chrom,
sowie als Rest Aluminium handelsüblicher Reinheit ent­hält.1. Aluminum alloy as a material for superplastic forming, characterized in that the alloy
0.8 - 2.5% iron,
3.5 - 6.0% magnesium,
0.1 - 0.6% manganese,
0.05 - 0.5% zircon,
Max. 6.0% zinc,
Max. 3.0% copper,
Max. 0.3% silicon,
Max. 0.05% titanium,
Max. 0.05% chromium,
as well as the rest contains aluminum of commercial purity. 2. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie 0,8 - 1,6 %, vorzugsweise 1,0 - 1,4 % Ei­sen enthält.2. Aluminum alloy according to claim 1, characterized in that it contains 0.8-1.6%, preferably 1.0-1.4% iron. 3. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie 4,0 - 5,0 % Magnesium enthält.3. Aluminum alloy according to claim 1, characterized in that it contains 4.0 - 5.0% magnesium. 4. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie 0,1 - 0,3 % Mangan enthält.4. Aluminum alloy according to claim 1, characterized in that it contains 0.1-0.3% manganese. 5. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie 0,1 - 0,2 % Zirkon enthält.5. Aluminum alloy according to claim 1, characterized in that it contains 0.1-0.2% zircon. 6. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie max. 0,15 % Silicium enthält.6. aluminum alloy according to claim 1, characterized in that it max. Contains 0.15% silicon. 7. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie 3,0 bis 4,0 % Zink enthält.7. Aluminum alloy according to claim 1, characterized in that it contains 3.0 to 4.0% zinc. 8. Aluminiumlegierung nach Anspruch 1, dadurch gekennzeich­net, dass sie
1,1 - 1,3 % Eisen,
4,3 - 4,7 % Magnesium,
0,1 - 0,3 % Mangan,
0,1 - 0,2 % Zirkon,
max. 0,15 % Silicium,
max. 0,05 % Titan,
max. 0,05 % Chrom,
sowie als Rest Aluminium handelsüblicher Reinheit ent­hält.8. Aluminum alloy according to claim 1, characterized in that it
1.1 - 1.3% iron,
4.3 - 4.7% magnesium,
0.1 - 0.3% manganese,
0.1 - 0.2% zircon,
Max. 0.15% silicon,
Max. 0.05% titanium,
Max. 0.05% chromium,
as well as the rest contains aluminum of commercial purity. 9. Verfahren zur Herstellung eines superplastisch umformba­ren Bleches aus einer Aluminiumlegierung nach einem der Ansprüche 1 bis 8 durch Giessen, Warm- und Kaltwalzen, wobei gegebenenfalls zwischen zwei Kaltwalzschritten eine Zwischenglühung durchgeführt wird, dadurch gekenn­zeichnet, dass der Verformungsgrad beim Kaltwalzen auf Enddicke, nach allfällig erfolgter Zwischenglühung, min­destens 60 %, vorzugsweise mindestens 70 %, beträgt.9. A method for producing a superplastic formable sheet from an aluminum alloy according to one of claims 1 to 8 by casting, hot and cold rolling, an intermediate annealing optionally being carried out between two cold rolling steps, characterized in that the degree of deformation during cold rolling to the final thickness, after any intermediate annealing, at least 60%, preferably at least 70%.
EP88810378A 1987-06-23 1988-06-09 Aluminium alloy for superplastic deformation Expired - Lifetime EP0297035B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88810378T ATE70566T1 (en) 1987-06-23 1988-06-09 ALUMINUM ALLOY FOR SUPER PLASTIC FORMING.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH2359/87 1987-06-23
CH235987 1987-06-23

Publications (2)

Publication Number Publication Date
EP0297035A1 true EP0297035A1 (en) 1988-12-28
EP0297035B1 EP0297035B1 (en) 1991-12-18

Family

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Family Applications (1)

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EP88810378A Expired - Lifetime EP0297035B1 (en) 1987-06-23 1988-06-09 Aluminium alloy for superplastic deformation

Country Status (5)

Country Link
US (1) US4874578A (en)
EP (1) EP0297035B1 (en)
AT (1) ATE70566T1 (en)
DE (1) DE3866969D1 (en)
NO (1) NO171171C (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0462056A1 (en) * 1990-06-11 1991-12-18 Alusuisse-Lonza Services Ag Aluminium alloy superplastic strip
EP0486426A1 (en) * 1990-11-12 1992-05-20 Alusuisse-Lonza Services AG Superplastic fabrication of work pieces
DE102014102254A1 (en) * 2014-02-21 2015-08-27 Dr. Ing. H.C. F. Porsche Aktiengesellschaft Method of manufacturing a fuel tank and fuel tank
US11421305B2 (en) 2016-04-19 2022-08-23 Rheinfelden Alloys Gmbh & Co. Kg Cast alloy

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0699789B2 (en) * 1989-02-23 1994-12-07 住友軽金属工業株式会社 Method for manufacturing high-strength aluminum alloy hard plate with excellent corrosion resistance
FR2645546B1 (en) * 1989-04-05 1994-03-25 Pechiney Recherche HIGH MODULATED AL MECHANICAL ALLOY WITH HIGH MECHANICAL RESISTANCE AND METHOD FOR OBTAINING SAME
WO1994006162A1 (en) * 1992-09-04 1994-03-17 N.F.A. - Energy And Ecology Industries Ltd. A method of manufacture of a chemical current source
US6322646B1 (en) 1997-08-28 2001-11-27 Alcoa Inc. Method for making a superplastically-formable AL-Mg product
US6253588B1 (en) 2000-04-07 2001-07-03 General Motors Corporation Quick plastic forming of aluminum alloy sheet metal
DE102017113216A1 (en) 2017-06-15 2018-12-20 Zollern Bhw Gleitlager Gmbh & Co. Kg Monotectic aluminum plain bearing alloy and process for its production and thus manufactured sliding bearing
CN111850351A (en) * 2020-07-01 2020-10-30 吉林大学 Method for preparing high-elongation cast-rolling Al-Mn series aluminum alloy plate blank

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DE2242235A1 (en) * 1971-08-28 1973-03-08 Showa Denko Kk SUPERPLASTIC ALLOY
FR2214755A1 (en) * 1973-01-19 1974-08-19 British Aluminium Co Ltd
US4021271A (en) * 1975-07-07 1977-05-03 Kaiser Aluminum & Chemical Corporation Ultrafine grain Al-Mg alloy product

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Publication number Priority date Publication date Assignee Title
DE2242235A1 (en) * 1971-08-28 1973-03-08 Showa Denko Kk SUPERPLASTIC ALLOY
FR2214755A1 (en) * 1973-01-19 1974-08-19 British Aluminium Co Ltd
US4021271A (en) * 1975-07-07 1977-05-03 Kaiser Aluminum & Chemical Corporation Ultrafine grain Al-Mg alloy product

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JOURNAL OF MATERIALS SCIENCE, Band 22, Nr. 1, 1987, Seiten 137-143, Chapman and Hall Ltd; A. JUHASZ et al.: "Superplasticity of aluminium alloys grain-refined by zirconium" *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0462056A1 (en) * 1990-06-11 1991-12-18 Alusuisse-Lonza Services Ag Aluminium alloy superplastic strip
US5122196A (en) * 1990-06-11 1992-06-16 Alusuisse-Lonza Services Ltd. Superplastic sheet metal made from an aluminum alloy
CH682326A5 (en) * 1990-06-11 1993-08-31 Alusuisse Lonza Services Ag
EP0486426A1 (en) * 1990-11-12 1992-05-20 Alusuisse-Lonza Services AG Superplastic fabrication of work pieces
CH682081A5 (en) * 1990-11-12 1993-07-15 Alusuisse Lonza Services Ag
DE102014102254A1 (en) * 2014-02-21 2015-08-27 Dr. Ing. H.C. F. Porsche Aktiengesellschaft Method of manufacturing a fuel tank and fuel tank
US11421305B2 (en) 2016-04-19 2022-08-23 Rheinfelden Alloys Gmbh & Co. Kg Cast alloy

Also Published As

Publication number Publication date
EP0297035B1 (en) 1991-12-18
NO882735L (en) 1988-12-27
NO171171B (en) 1992-10-26
NO171171C (en) 1993-02-03
DE3866969D1 (en) 1992-01-30
NO882735D0 (en) 1988-06-21
ATE70566T1 (en) 1992-01-15
US4874578A (en) 1989-10-17

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