EP0320417A1 - Mechanical parts, such as piston connecting rods, made from an aluminium alloy with improved fatigue resistance, and process for their manufacture - Google Patents

Mechanical parts, such as piston connecting rods, made from an aluminium alloy with improved fatigue resistance, and process for their manufacture Download PDF

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Publication number
EP0320417A1
EP0320417A1 EP88420409A EP88420409A EP0320417A1 EP 0320417 A1 EP0320417 A1 EP 0320417A1 EP 88420409 A EP88420409 A EP 88420409A EP 88420409 A EP88420409 A EP 88420409A EP 0320417 A1 EP0320417 A1 EP 0320417A1
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Prior art keywords
connecting rods
alloy
manufacture
parts
aluminium alloy
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EP88420409A
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German (de)
French (fr)
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EP0320417B1 (en
Inventor
Jean-François Faure
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Constellium Issoire SAS
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Cegedur Societe de Transformation de lAluminium Pechiney SA
Pechiney Rhenalu SAS
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Priority to AT88420409T priority Critical patent/ATE66023T1/en
Publication of EP0320417A1 publication Critical patent/EP0320417A1/en
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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
    • 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
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent

Definitions

  • the present invention relates to aluminum alloy parts having improved fatigue resistance and to a method for manufacturing said parts.
  • EP 144 898 teaches an aluminum alloy containing by weight 10 to 36% of silicon, 1 to 12% of copper, 0.1 to 3% of magnesium and 2 to 10% at least an element chosen from the group Fe, Ni, Co, Cr and Mn.
  • This alloy is applicable to the manufacture of parts intended for both the aeronautical and automotive industries, said parts being obtained by the technique of powder metallurgy comprising, in addition to shaping by compacting and spinning, an intermediate processing step thermal between 250 and 550 ° C.
  • this alloying element added to the others in an amount at least equal to 0.4% to have a suitable effect but not exceeding 1.5%, quantity beyond which the 'improvement obtained is no longer noticeable, had the consequence of increasing the fatigue resistance of the parts and this without harming either the other properties obtained with the alloys of the prior art, nor their ability to be machined.
  • the invention also relates to a process for obtaining parts from such alloys.
  • the parts after being possibly subjected to machining, are heat treated between 480 and 530 ° C for 1 to 10 hours, then quenched in water before undergoing a tempering treatment between 150 and 200 ° C for 2 to 32 hours, which improves their mechanical characteristics.
  • Alloys n ° 1, 2 and 3 were obtained by powder metallurgy, i.e. they were melted at 900 ° C and then atomized in a nitrogen atmosphere in the form of particle size 300 ⁇ m then compacted under 300 MPa in an isostatic press, spun in the form of a bar with a diameter of 40 mm.
  • the technique used was that of the "spray deposition" during which a deposit was obtained in the form of a cylindrical billet which was then transformed by spinning into a bar of diameter 40 mm. The bars originating from one or the other process were then treated for 2 hours between 490 and 520 ° C.

Abstract

Aluminium alloy articles with an improved fatigue strength and process for their manufacture. <??>These articles are made of an alloy containing, by weight, 11 to 22% of silicon, 2 to 5% of iron, 0.5 to 4% of copper, 0.2 to 1.5% of magnesium, having a characteristic of containing 0.4 to 1.5% of zirconium. <??>The manufacturing process consists in subjecting the alloy in molten state to a means for fast solidification, in forming it, in subjecting it to a heat treatment between 480 and 530 DEG C followed by a water quenching and by annealing between 150 and 200 DEG C. <??>These articles find their application especially in the form of connecting rods and gudgeon pins.

Description

La présente invention est relative à des pièces en alliage d'aluminium ayant une résistance à la fatigue améliorée et à un procédé de fabrication desdites pièces.The present invention relates to aluminum alloy parts having improved fatigue resistance and to a method for manufacturing said parts.

On sait que l'aluminium a notamment pour propriétés d'être trois fois plus léger que l'acier et d'avoir une bonne résistance à la corrosion. En l'alliant à des métaux tels que le cuivre et le magnésium, on améliore fortement sa résistance mécanique. Par ailleurs, l'ajout de silicium donne un produit ayant une bonne résistance à l'usure. Ces alliages dopés avec d'autres éléments tels que le fer, le nickel, le cobalt, le chrome et le manganèse, conduisent à un compromis de propriétés qui en font un matériau de choix pour la fabrication de pièces pour automobiles telles que moteur, piston, cylindre, etc...We know that aluminum has the particular properties of being three times lighter than steel and of having good corrosion resistance. By combining it with metals such as copper and magnesium, its mechanical resistance is greatly improved. Furthermore, the addition of silicon gives a product having good wear resistance. These alloys doped with other elements such as iron, nickel, cobalt, chromium and manganese, lead to a compromise of properties which make it a material of choice for the manufacture of parts for automobiles such as engine, piston , cylinder, etc ...

C'est ainsi que l'EP 144 898 enseigne un alliage d'aluminium contenant en poids 10 à 36 % de silicium, 1 à 12 % de cuivre, 0,1 à 3 % de magnésium et 2 à 10 % d'au moins un élément choisi dans le groupe Fe, Ni, Co, Cr et Mn.This is how EP 144 898 teaches an aluminum alloy containing by weight 10 to 36% of silicon, 1 to 12% of copper, 0.1 to 3% of magnesium and 2 to 10% at least an element chosen from the group Fe, Ni, Co, Cr and Mn.

Cet alliage est applicable à la confection de pièces destinées aussi bien à l'industrie aéronautique qu'automobile, lesdites pièces étant obtenues par la technique de la métallurgie des poudres comportant, outre la mise en forme par compactage et filage, une étape intermédiaire de traitement thermique entre 250 et 550°C.This alloy is applicable to the manufacture of parts intended for both the aeronautical and automotive industries, said parts being obtained by the technique of powder metallurgy comprising, in addition to shaping by compacting and spinning, an intermediate processing step thermal between 250 and 550 ° C.

Si ces pièces répondent bien aux différentes propriétés énoncées ci-dessus, il en est une qui n'a pas encore été prise en compte, à savoir la tenue à la fatigue.
L'homme de l'art sait que la fatigue correspond à un changement permanent, localisé et progressif de la structure métallique qui se produit dans les matériaux soumis à une succession de contraintes discontinues et qui peut entraîner des fissures et même des ruptures des pièces après une application desdites contraintes suivant un nombre de cycles plus ou moins grand et ce alors que leur intensité est le plus souvent nettement inférieure à celle qu'il faut appliquer au matériau de façon continue pour obtenir une rupture par traction. C'est pourquoi les valeurs de module d'élasticité, de résistance à la traction, de dureté énoncées dans l'EP 144 898 ne peuvent rendre compte de l'aptitude de l'alliage à la résistance à la fatigue.If these parts respond well to the various properties set out above, there is one that has not yet been taken into account, namely fatigue resistance.
Those skilled in the art know that fatigue corresponds to a permanent, localized and gradual change in the metallic structure which occurs in materials subjected to a succession of discontinuous stresses and which can cause cracks and even ruptures of the parts after a application of said stresses according to a greater or lesser number of cycles and this while their intensity is most often significantly lower than that which must be applied to the material continuously to obtain a rupture by traction. This is why the values of modulus of elasticity, tensile strength, hardness stated in EP 144 898 cannot account for the suitability of the alloy for fatigue resistance.

Or, il est important pour des pièces telles que les bielles ou les axes de piston, par exemple qui travaillent en dynamique et qui sont soumises à des efforts périodiques, de présenter une bonne tenue à la fatigue.However, it is important for parts such as the connecting rods or the piston pins, for example which work dynamically and which are subjected to periodic forces, to have good resistance to fatigue.

C'est pourquoi la demanderesse s'étant penchée sur ce problème a constate que certes les pièces fabriquées à partir des alliages entrant dans le cadre du document sus-mentionné présentaient une résistance à la fatigue qui pouvait convenir à certaines applications, mais qu'il était possible d'améliorer notablement cette propriété en modifiant leur composition. C'est dans ce but qu'elle a mis au point des pièces en alliages d'aluminium contenant en poids 11 à 22 % de silicium, 2 à 5 % de fer, 0,5 à 4 % de cuivre, 0,2 à 1,5 % de magnésium caractérisées en ce qu'elles contiennent également 0,4 à 1,5 % de zirconium.This is why the Applicant, having looked into this problem, has observed that, admittedly, the parts made from alloys falling within the scope of the above-mentioned document had a resistance to fatigue which could be suitable for certain applications, but that it was possible to significantly improve this property by modifying their composition. It is for this purpose that it has developed parts in aluminum alloys containing by weight 11 to 22% of silicon, 2 to 5% of iron, 0.5 to 4% of copper, 0.2 to 1.5% magnesium, characterized in that it also contains 0.4 to 1.5% zirconium.

En effet, la demanderesse s'est aperçue que cet élément d'alliage ajouté aux autres en quantité au moins égale à 0,4 % pour avoir un effet convenable mais n'excédant pas 1,5 %, quantité au-delà de laquelle l'amélioration obtenue n'est plus sensible, avait pour conséquence d'accroître la résistance à la fatigue des pièces et ce sans nuire ni aux autres propriétés obtenues avec les alliages de l'art antérieur, ni à leur aptitude à l'usinage.Indeed, the Applicant has noticed that this alloying element added to the others in an amount at least equal to 0.4% to have a suitable effect but not exceeding 1.5%, quantity beyond which the 'improvement obtained is no longer noticeable, had the consequence of increasing the fatigue resistance of the parts and this without harming either the other properties obtained with the alloys of the prior art, nor their ability to be machined.

L'invention concerne également un procédé d'obtention des pièces à partir de tels alliages.The invention also relates to a process for obtaining parts from such alloys.

Il consiste après avoir élaboré l'alliage de composition revendiquée, à le fondre à une température supérieure à 900°C de manière à éviter tout phénomène de précipitation prématuré puis à le soumettre à un moyen de solidification rapide. En effet, comme les éléments tels que le fer et le zirconium sont très peu solubles dans l'alliage, il est indispensable pour obtenir des pièces répondant aux caractéristiques souhaitées d'éviter une précipitation grossière et hétérogène de ces éléments ce qu'on réalise en les refroidissant le plus rapidement possible.It consists, after having developed the alloy of the claimed composition, in melting it at a temperature above 900 ° C. so as to avoid any phenomenon of premature precipitation and then in subjecting it to a means of rapid solidification. Indeed, as elements such as iron and zirconium are very poorly soluble in the alloy, it is essential to obtain parts meeting the desired characteristics to avoid a coarse and heterogeneous precipitation of these elements which is achieved by cooling them as quickly as possible.

Il existe plusieurs façons d'opérer cette solidification rapide :
- soit par atomisation du métal fondu à l'aide d'un gaz ou par atomisation mécanique suivie d'un refroidissement dans un gaz (air, hélium, argon); ce qui conduit à des poudres de granulométrie inférieure à 400 µm qui sont ensuite mis en forme par compactage à froid ou à chaud, dans une presse uniaxiale ou isostatique puis filage et/ou forgeage;
- soit par projection de l'alliage fondu contre une surface métallique refroidie, technique désignée par les Anglo-Saxons sous l'expression "melt spinning", ou "planar flow casting" et dont on trouve des descriptions dans les brevets US 4.389.258 et EP 136.508, ce qui génère des rubans d'épaisseur inférieure à 100 µm qui sont ensuite mises en forme par compactage comme ci-dessus;
- soit encore par projection de l'alliage fondu atomisé dans un courant de gaz contre un substrat, technique encore appelée "spray deposition" dont un exemple est donné dans le brevet GB 1.379.261, et qui conduit à un dépôt cohérent suffisamment malléable pour être mis en forme par forgeage, filage ou matriçage par exemple.There are several ways to operate this rapid solidification:
- either by atomization of the molten metal using a gas or by mechanical atomization followed by cooling in a gas (air, helium, argon); which leads to powders with a particle size of less than 400 μm which are then shaped by cold or hot compaction, in a uniaxial or isostatic press then spinning and / or forging;
- Either by projection of the molten alloy against a cooled metallic surface, a technique designated by the Anglo-Saxons under the expression "melt spinning", or "planar flow casting" and of which descriptions are found in US Patents 4,389,258 and EP 136,508, which generates ribbons of thickness less than 100 μm which are then shaped by compacting as above;
- Or again by projection of the molten alloy atomized in a stream of gas against a substrate, a technique also called "spray deposition", an example of which is given in patent GB 1,379,261, and which leads to a coherent deposit which is sufficiently malleable for be shaped by forging, spinning or stamping for example.

Cette liste est bien entendu non exhaustive.This list is of course not exhaustive.

Afin d'affiner davantage la structure de précipitation, les pièces après avoir été soumises éventuellement à un usinage sont traitées thermiquement entre 480 et 530°C pendant 1 à 10 heures, puis trempées à l'eau avant de subir un traitement de revenu entre 150 et 200°C pendant 2 à 32 heures, ce qui améliore leurs caractéristiques mécaniques.In order to further refine the precipitation structure, the parts, after being possibly subjected to machining, are heat treated between 480 and 530 ° C for 1 to 10 hours, then quenched in water before undergoing a tempering treatment between 150 and 200 ° C for 2 to 32 hours, which improves their mechanical characteristics.

L'invention sera mieux comprise à l'aide des exemples d'application suivants:The invention will be better understood using the following application examples:

Six alliages ont été mis en oeuvre. Il avaient la composition suivante en poids : Alliage N° Si % Fe % Cu % Mg % Zr % Al % 1 18 3,0 3 1,0 - reste 2 18 3,0 3 1,0 1 reste 3 12 5,0 1 1,5 1,2 reste 4 15 4,0 1 1 0,6 reste 5 20 4,0 1 1 0,8 reste 6 12 5,0 3 0,8 0,2 reste Six alloys have been used. They had the following composition by weight: Alloy No. Yes % Fe% Cu% Mg% Zr% Al% 1 18 3.0 3 1.0 - rest 2 18 3.0 3 1.0 1 rest 3 12 5.0 1 1.5 1.2 rest 4 15 4.0 1 1 0.6 rest 5 20 4.0 1 1 0.8 rest 6 12 5.0 3 0.8 0.2 rest

Les alliages n°1, 2 et 3 ont été obtenus par métallurgie des poudres, c'est-à-dire qu'ils ont été ont été fondus à 900°C puis atomisés dans une atmosphère d'azote sous forme de particules de granulométrie 300 µm puis compactés sous 300 MPa dans une presse isostatique, filés sous forme de barre de diamètre 40 mm.
Pour les alliages N° 4, 5 et 6, la technique utilisée était celle de la "spray déposition" au cours de laquelle on a obtenu un dépôt sous forme d'une billette cylindrique qui a été ensuite transformée par filage en barre de diamètre 40 mm. Les barres provenant de l'un ou l'autre procédé ont ensuite été traitées pendant 2 heures entre 490 et 520°C puis trempées à l'eau et soumises pendant 8 heures à une température comprise entre 160 et190°C.
On a effectué sur des éprouvettes de chacune d'elles des mesures d'une part du module d'Young, d'autre part de la limite élastique conventionnelle à 0,2 %, la charge de rupture et l'allongement successivement à 20°C et à 150°C après 100 heures de maintien, ainsi que les mesures de la limite de fatigue à 20°C au bout de 10⁷ cycles et du rapport d'endurance, défini par le rapport entre la limite d'endurance et la charge de rupture.Alloys n ° 1, 2 and 3 were obtained by powder metallurgy, i.e. they were melted at 900 ° C and then atomized in a nitrogen atmosphere in the form of particle size 300 µm then compacted under 300 MPa in an isostatic press, spun in the form of a bar with a diameter of 40 mm.
For alloys 4, 5 and 6, the technique used was that of the "spray deposition" during which a deposit was obtained in the form of a cylindrical billet which was then transformed by spinning into a bar of diameter 40 mm. The bars originating from one or the other process were then treated for 2 hours between 490 and 520 ° C. then quenched with water and subjected for 8 hours at a temperature between 160 and 190 ° C.
We carried out on test pieces of each of them measurements on the one hand of the Young's modulus, on the other hand of the conventional elastic limit at 0.2%, the breaking load and the elongation successively at 20 ° C and at 150 ° C after 100 hours of maintenance, as well as the fatigue limit measurements at 20 ° C after 10⁷ cycles and the endurance ratio, defined by the ratio between the endurance limit and the load a break.

Les résultats figurent dans le tableau suivant : 1 2 3 4 5 6 Module d'Young en GPa 87 91 89 90 95 84 Traction à 20°C RO,2 en MPa 350 390 380 387 400 355 Rm en MPa 430 460 442 455 470 433 A% 2,5 3,0 5,0 3,8 1,0 2,0 Traction à 150°C RO,2 en MPa 290 320 315 323 327 288 après 100 h de Rm en MPa 385 390 387 393 398 380 maintien A% 5,0 6,0 8,0 5,0 2,0 6,0 Limite de fatigue Lf en MPa à 10⁷ cycles à 20°C (flexion rotative) 150 185 192 190 188 155 Rapport d'endurance (Lf/Rm) 0,35 0,40 0,43 0,42 0,40 0,36 The results are shown in the following table: 1 2 3 4 5 6 Young's modulus in GPa 87 91 89 90 95 84 Traction at 20 ° C RO, 2 in MPa 350 390 380 387 400 355 Rm in MPa 430 460 442 455 470 433 AT% 2.5 3.0 5.0 3.8 1.0 2.0 Traction at 150 ° C RO, 2 in MPa 290 320 315 323 327 288 after 100 h of Rm in MPa 385 390 387 393 398 380 hold A% 5.0 6.0 8.0 5.0 2.0 6.0 Fatigue limit Lf in MPa at 10⁷ cycles at 20 ° C (rotary bending) 150 185 192 190 188 155 Endurance ratio (Lf / Rm) 0.35 0.40 0.43 0.42 0.40 0.36

On constate la nette amélioration apportée par le zirconium sur la résistance à la fatigue, qui passe d'une limite de 150 à 192 MPa.We note the clear improvement brought by zirconium on the resistance to fatigue, which goes from a limit of 150 to 192 MPa.

Des résultats analogues ont été obtenus sur des pièces obtenues par "spray deposition" et "melt spinning" ou "planar flow casting".Similar results have been obtained on parts obtained by "spray deposition" and "melt spinning" or "planar flow casting".

Claims (3)

1. Pièces en alliage d'aluminium, telles que bielles notamment, ayant une résistance à la fatigue améliorée qui, outre l'aluminium, contient en poids 11 à 22 % de silicium, 2 à 5 % de fer, 0,5 à 4 % de cuivre, 0,2 à 1,5 % de magnésium, caractérisées en ce qu'elles contiennent également 0,4 à 1,5 % de zirconium.1. Parts of aluminum alloy, such as connecting rods in particular, having an improved resistance to fatigue which, in addition to aluminum, contains by weight 11 to 22% of silicon, 2 to 5% of iron, 0.5 to 4 % copper, 0.2 to 1.5% magnesium, characterized in that they also contain 0.4 to 1.5% zirconium. 2. Procédé d'obtention de pièces suivant la revendication 1 caractérisé en ce que l'on soumet l'alliage à l'état fondu à un moyen de solidification rapide, le met en forme, lui fait subir un traitement thermique entre 480 et 530°C, le trempe à l'eau et effectue un revenu entre 150 et 200°C.2. Method for obtaining parts according to claim 1 characterized in that the alloy is subjected to the molten state to a rapid solidification means, it is shaped, it is subjected to a heat treatment between 480 and 530 ° C, quench with water and effect an income between 150 and 200 ° C. 3. Procédé selon la revendication 2 caractérisé en ce que le moyen de solidification rapide appartient au groupe constitué par l'atomisation, la "spray deposition" et le "melt spinning".3. Method according to claim 2 characterized in that the rapid solidification means belongs to the group consisting of atomization, the "spray deposition" and the "melt spinning".
EP88420409A 1987-12-07 1988-12-05 Mechanical parts, such as piston connecting rods, made from an aluminium alloy with improved fatigue resistance, and process for their manufacture Expired - Lifetime EP0320417B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88420409T ATE66023T1 (en) 1987-12-07 1988-12-05 MACHINERY PARTS SUCH AS CONNECTING RODS AND LIKE MADE OF ALUMINUM ALLOY WITH INCREASED FATIGUE RESISTANCE AND PROCESS FOR THEIR MANUFACTURE.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8717674A FR2624137B1 (en) 1987-12-07 1987-12-07 ALUMINUM ALLOY PARTS, SUCH AS CONNECTING RODS, WITH IMPROVED FATIGUE RESISTANCE AND METHOD OF MANUFACTURE
FR8717674 1987-12-07

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EP0320417A1 true EP0320417A1 (en) 1989-06-14
EP0320417B1 EP0320417B1 (en) 1991-08-07

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US (1) US4923676A (en)
EP (1) EP0320417B1 (en)
JP (1) JPH0617550B2 (en)
KR (1) KR890010260A (en)
CN (1) CN1034585A (en)
AT (1) ATE66023T1 (en)
BR (1) BR8806421A (en)
DD (1) DD276109A5 (en)
DE (1) DE3864128D1 (en)
DK (1) DK679288A (en)
ES (1) ES2024044B3 (en)
FI (1) FI885657A (en)
FR (1) FR2624137B1 (en)
HU (1) HUT50885A (en)
IL (1) IL88586A0 (en)
PL (1) PL276247A1 (en)
SU (1) SU1722234A3 (en)
YU (1) YU220988A (en)

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DE69221690T2 (en) * 1991-04-03 1998-04-02 Sumitomo Electric Industries ROTOR FOR OIL PUMP FROM AN ALUMINUM ALLOY AND ITS PRODUCTION METHOD
JP3021487U (en) * 1995-08-08 1996-02-20 株式会社スリーリング Car armrest cover
EP0864660B1 (en) * 1997-02-12 2003-05-14 Yamaha Hatsudoki Kabushiki Kaisha Piston for internal combustion engine and method for producing same
US7699595B2 (en) * 2004-07-19 2010-04-20 R + S Technik Gmbh Method and apparatus for molding a laminated trim component without use of slip frame
CN101775530B (en) * 2010-03-04 2012-03-28 安徽省恒泰动力科技有限公司 Hypereutectic al-si alloy piston material
US10531545B2 (en) 2014-08-11 2020-01-07 RAB Lighting Inc. Commissioning a configurable user control device for a lighting control system
CN106756293B (en) * 2016-12-20 2019-03-01 江苏豪然喷射成形合金有限公司 A kind of preparation method of ferro-silicon-aluminium copper magnesium alloy
CN107377973A (en) * 2017-08-30 2017-11-24 广东美芝制冷设备有限公司 Alloy components and its preparation method and application
CN108715957A (en) * 2018-05-31 2018-10-30 益阳仪纬科技有限公司 A kind of automotive transmission shell high-strength aluminum alloy composite material and its preparation process
DE102018117418A1 (en) * 2018-07-18 2020-01-23 Friedrich Deutsch Metallwerk Gesellschaft M.B.H. Die-cast aluminum alloy

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GB388109A (en) * 1930-10-03 1933-02-23 Skoda Works Plzen Ltd Company Aluminium alloys for pistons
US1921195A (en) * 1931-07-14 1933-08-08 Aluminum Co Of America Aluminum silicon alloy
GB563617A (en) * 1941-12-04 1944-08-23 Fairweather Harold G C Improvements in or relating to aluminium base alloys
EP0144898A2 (en) * 1983-12-02 1985-06-19 Sumitomo Electric Industries Limited Aluminum alloy and method for producing same

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Publication number Priority date Publication date Assignee Title
GB388109A (en) * 1930-10-03 1933-02-23 Skoda Works Plzen Ltd Company Aluminium alloys for pistons
US1921195A (en) * 1931-07-14 1933-08-08 Aluminum Co Of America Aluminum silicon alloy
GB563617A (en) * 1941-12-04 1944-08-23 Fairweather Harold G C Improvements in or relating to aluminium base alloys
EP0144898A2 (en) * 1983-12-02 1985-06-19 Sumitomo Electric Industries Limited Aluminum alloy and method for producing same

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DK679288A (en) 1989-06-08
DE3864128D1 (en) 1991-09-12
CN1034585A (en) 1989-08-09
ATE66023T1 (en) 1991-08-15
PL276247A1 (en) 1989-06-12
ES2024044B3 (en) 1992-02-16
KR890010260A (en) 1989-08-07
FI885657A0 (en) 1988-12-05
IL88586A0 (en) 1989-07-31
SU1722234A3 (en) 1992-03-23
HUT50885A (en) 1990-03-28
EP0320417B1 (en) 1991-08-07
FR2624137B1 (en) 1990-06-15
FI885657A (en) 1989-06-08
JPH0617550B2 (en) 1994-03-09
JPH01198444A (en) 1989-08-10
YU220988A (en) 1990-04-30
FR2624137A1 (en) 1989-06-09
DK679288D0 (en) 1988-12-06
DD276109A5 (en) 1990-02-14
US4923676A (en) 1990-05-08
BR8806421A (en) 1989-08-22

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