EP0196984A1 - Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture - Google Patents
Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture Download PDFInfo
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- EP0196984A1 EP0196984A1 EP86420062A EP86420062A EP0196984A1 EP 0196984 A1 EP0196984 A1 EP 0196984A1 EP 86420062 A EP86420062 A EP 86420062A EP 86420062 A EP86420062 A EP 86420062A EP 0196984 A1 EP0196984 A1 EP 0196984A1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/08—Amorphous alloys with aluminium as the major constituent
Definitions
- the invention relates to alloys based on Al. essentially containing Ni and / or Fe. of Si as main alloying elements, obtained in the essentially amorphous state, by relatively rapid solidification.
- essentially amorphous is meant an alloy in which the crystallized volume fraction is at most equal to 25%.
- Ni can be partially substituted by Fe up to 10% by V or B (up to 5 at%) or completely by Mn (up to 22% at%), the rest being made up of 'Al and usual processing impurities.
- alloys have a set of remarkable properties in the amorphous or essentially amorphous state as well as in the microcrystallized state obtained by annealing of the amorphous or essentially amorphous state. These properties result from the introduction of a large quantity of alloying elements without rhedibitory effects of segregation or of the formation of fragile intermetallic phases of dimensions greater than 10 ⁇ m.
- the unique combination of compositions and structures thus obtained gives these alloys high hardnesses, excellent heat stability for long-term annealing as well as special tribological properties.
- a consolidation process consists of grinding the ribbons obtained by casting on a wheel, sieving below 100 ⁇ m, hot compression between 350 and 400 ° C and hot spinning around 400-450 ° C. It is thus possible to obtain massive products.
- the essentially amorphous alloy according to the invention therefore exhibits very good friction and abrasion behavior.
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Abstract
Description
L'invention se rapporte à des alliages base d'Al. contenant essentiellement du Ni et/ou du Fe. du Si comme éléments d'alliages principaux, obtenus à l'état essentiellement amorphe, par solidification relativement rapide. Par essentiellement amorphe, on entend un alliage dans lequel la fraction volumique cristallisée est au plus égale à 25 %.The invention relates to alloys based on Al. essentially containing Ni and / or Fe. of Si as main alloying elements, obtained in the essentially amorphous state, by relatively rapid solidification. By essentially amorphous is meant an alloy in which the crystallized volume fraction is at most equal to 25%.
Bien que les alliages amorphes à base d'Al soient déjà connus de façon globale (voir la demande de brevet français n° 2 529 909), leur obtention pratique et industrielle se heurte à de grandes difficultés, en raison des paramètres de fabrication extrêmement étroits à respecter pour l'obtention de la structure essentiellement amorphe.Although the amorphous alloys based on Al are already generally known (see French patent application No. 2,529,909), their practical and industrial production encounters great difficulties, due to the extremely narrow manufacturing parameters. to be observed for obtaining the essentially amorphous structure.
Ces paramètres sont principalement l'intervalle de température "de trempe" depuis l'état liquide ainsi que la vitesse minimale de solidification.These parameters are mainly the temperature range "quenching" from the liquid state as well as the minimum rate of solidification.
Le développement industriel de tels alliages est donc conditionné par la sélection d'alliages présentant un intervalle de trempe suffisamment large (environ 100°C entre la température de l'alliage liquide et le liquidus de celui-ci) et des vitesses de solidification pas trop rapides (de l'ordre de 104 K/sec.).The industrial development of such alloys is therefore conditioned by the selection of alloys having a sufficiently wide quenching interval (approximately 100 ° C. between the temperature of the liquid alloy and the liquidus thereof) and not too solidification rates. fast (of the order of 10 4 K / sec.).
Seul un petit nombre d'alliages selon l'invention répond à ces objectifs. Ces alliages contiennent (en atome %) :Only a small number of alloys according to the invention meets these objectives. These alloys contain (in atom%):
- de 5 à 30 % de Sifrom 5 to 30% of Si
- de 11 à 22 % de Ni11 to 22% Ni
- Fe + Ni + Si ≦ 42 %Fe + Ni + Si ≦ 4 2%
le (Ni) pouvant être partiellement substitué par le Fe jusqu'à 10% par le V ou le B (jusqu'à 5 at %) ou totalement par le Mn (jusqu'à 22% at %), le reste étant constitué d'Al et des impuretés d'élaboration habituelles.(Ni) can be partially substituted by Fe up to 10% by V or B (up to 5 at%) or completely by Mn (up to 22% at%), the rest being made up of 'Al and usual processing impurities.
Les alliages contiennent de préferénce :
- de 9 à 25% de Si
- de 11 à 19 % de Ni
- avec 21 ≦ Fe + Ni + Si ≦ 38 %
le manganèse étant limité à 5 at. %.The alloys contain preferably:
- from 9 to 25% of Si
- 11 to 19% Ni
- with 21 ≦ Fe + Ni + Si ≦ 38%
manganese being limited to 5 at. %.
Dans ces conditions, il est possible d'obtenir des alliages industriels amorphes de façon reproductible.Under these conditions, it is possible to obtain reproducible amorphous industrial alloys.
Ces alliages présentent un ensemble de propriétés remarquables dans l'état amorphe ou essentiellement amorphe aussi bien que dans l'état microcristallisé obtenu par recuit de l'état amorphe ou essentieltement amorphe. Ces propriétés résultent de l'introduction d'une quantité importante d'éléments d'alliage sans effets rhédibitoires de ségrégation ou de formation de phases intermétalliques fragiles de dimensions supérieures à 10 µm. La combinaison unique des compositions et des structures ainsi obtenue confère à ces alliages des duretés élevées, une excellente stabilité à chaud pour des recuits de longue durée ainsi que des propriétés tribologiques particulières.These alloys have a set of remarkable properties in the amorphous or essentially amorphous state as well as in the microcrystallized state obtained by annealing of the amorphous or essentially amorphous state. These properties result from the introduction of a large quantity of alloying elements without rhedibitory effects of segregation or of the formation of fragile intermetallic phases of dimensions greater than 10 μm. The unique combination of compositions and structures thus obtained gives these alloys high hardnesses, excellent heat stability for long-term annealing as well as special tribological properties.
La possibilité d'obtenir des structures essentiellement amorphes pour des vitesses de solidification de l'ordre de 104 K/sec. permet d'utiliser différents procédés d'obtention de ces alliages. C'est ainsi qu'outre les procédés de trempe rapide sur roue ou d'atomisation gazeuse on peut utiliser un dépôt plasma de poudres préalliées sur un substrat métallique (ou bon conducteur de la chaleur tel que le graphite) ou encore le nickelage superficiel chimique ou électrochimique d'un alliage d'Al contenant du Si (type AS), de préférence entre 10 et 25% de Si. suivi d'une fusion du dépôt de nickel et d'une partie du substrat au moyen d'une source de chaleur concentrée et localisée tefle que laser, torche plasma, chauffage HF, torche TIG, etc...The possibility of obtaining essentially amorphous structures for solidification rates of the order of 10 4 K / sec. allows the use of different processes for obtaining these alloys. Thus, in addition to the rapid quenching processes on a wheel or gas atomization, it is possible to use a plasma deposition of pre-alloyed powders on a metal substrate (or good conductor of heat such as graphite) or even chemical surface nickel plating. or electrochemical of an Al alloy containing Si (AS type), preferably between 10 and 25% of Si. followed by a fusion of the nickel deposit and part of the substrate by means of a source of concentrated and localized heat such as laser, plasma torch, HF heating, TIG torch, etc ...
Un procédé de consolidation consiste en un broyage des rubans obtenus par coulée sur roue, en un tamisage au-dessous de 100 µm, une compression à chaud entre 350 et 400°C et en un filage à chaud vers 400-450°C. Il est ainsi possible d'obtenir des produits massifs.A consolidation process consists of grinding the ribbons obtained by casting on a wheel, sieving below 100 µm, hot compression between 350 and 400 ° C and hot spinning around 400-450 ° C. It is thus possible to obtain massive products.
L'invention sera mieux comprise à l'aide des exemples décrits ci-après et des figures suivantes :
- . Les figures 1 à 3 donnent respectivement les diagrammes de diffraction aux rayons X, d'un alliage amorphe, essentiellement amorphe (environ 20 % à l'état cristallisé) et microcristallin.
- . La figure 4 représente les limites de composition des alliages Al Ni Si, selon l'invention.
- . La figure 5 représente l'évolution des microàuretés Vickers de deux alliages initialement amorphes : Al70Ni15Si22Mn13 et Al70Ni15Si15 après des maintiens d'une heure à diverses températures.
- . La figure 6 est un diffractogramme de l'alliage Al70 Ni15Si15 déposé par plasma atmosphérique et obtenu avec la radiation Cu K a.
- . La figure 7 représente les pertes de poids (AP) observées sur un revêtement Al70 Ni15Si15 comparativement à un alliage A-S17U4G, reconnu comme résistant à l'usure, en fonction du nombre de cycles (N) sur abrasimètre TABER.
- . FIGS. 1 to 3 respectively give the X-ray diffraction diagrams of an amorphous, essentially amorphous (about 20% in the crystallized state) and microcrystalline alloy.
- . FIG. 4 represents the limits of composition of the Al Ni Si alloys according to the invention.
- . FIG. 5 represents the evolution of the Vickers micro-hardnesses of two initially amorphous alloys: Al 70 Ni 15 Si 22 Mn 13 and Al 70 Ni 15 Si 15 after one hour maintenance at various temperatures.
- . FIG. 6 is a diffractogram of the alloy Al 70 Ni 15 Si 15 deposited by atmospheric plasma and obtained with the Cu K a radiation.
- . FIG. 7 represents the weight losses (AP) observed on an Al 70 Ni 15 Si 15 coating compared to an alloy A-S17U4G, recognized as resistant to wear, as a function of the number of cycles (N) on a TABER abrasimeter.
Le Tableau 1 rassemble des exemples de compositions d'alliages amorphes définies dans le cadre de la présente invention et obtenues sous forme de rubans de 20 µm d'épaisseur par trempe sur une roue de Cu, la vitesse linéaire d'éjection du ruban étant de 60ms-1. La crishllisa- tion de ces alliages a été étudiée par analyse enthalpique différentielle, par rayons X, par microscopie électronique en transmission et par mesures de microduretés. La température du 1er pic de cristallisation est reportée au Tableau 1 pour chaque composition. Ainsi, pour l'alliage Al70Ni15Si15 cette température est de 190°C alors qu'elle est de 295°C pour l'alliage Al70Ni15Si12Mn3. Pour les alliages ternaires (Al2Ni2Si), cette température augmente :
- a) à teneur en Al constante, pour des teneurs croissantes en Ni
- b) pour des teneurs croissantes d'éléments d'alliage - (Ni+Si).
- a) with constant Al content, for increasing Ni contents
- b) for increasing contents of alloying elements - (Ni + Si).
La figure 5 montre l'évolution de la microdureté Vickers sous 10 g des rubans mesurée à 20°C après des recuits isothermes d'une heure à différentes températures. De façon générale, la cristallisation s'accompagne d'une importante augmentation de la dureté. On notera les niveaux élevés de microdureté obtenus (300HV à 560HV). Après recuit d'une heure à 200°C, l'alliage Al70Ni13Si17 présente une cristallisation abondante d'une nouvelle phase intermétallique métastable de structure hexagonale (a = 0,664nm, c = 0,377nm) avec un début de cristallisation de l'Al. Après une heure à 300°C l'alliage est constitué de micrograins d'Al, de Si et de phase Al3Ni orthorhombique d'équilibre.FIG. 5 shows the evolution of the Vickers microhardness under 10 g of the ribbons measured at 20 ° C. after isothermal annealing for one hour at different temperatures. Generally, crystallization is accompanied by a significant increase in hardness. Note the high levels of microhardness obtained (300HV to 560HV). After annealing for one hour at 200 ° C., the Al 70 Ni 13 Si 17 alloy exhibits abundant crystallization of a new metastable intermetallic phase of hexagonal structure (a = 0.664nm, c = 0.377nm) with the onset of crystallization. of Al. After one hour at 300 ° C., the alloy consists of micrograins of Al, Si and of equilibrium orthorhombic Al 3 Ni phase.
Les examens en microscopie optique et électronique en transmission montrent qu'après maintien d'une heure à 400°C, la taille moyenne des grains est comprise entre 0,05 um et 0,5 µm. Cette structure microcristalline très fine ne peut être obtenue pour de telles compositions que par recuit d'un alliage amorphe et confère à l'alliage à la fois des résistances mécaniques et des ductilités élevées.The examinations in optical and transmission electron microscopy show that after maintaining one hour at 400 ° C, the average grain size is between 0.05 µm and 0.5 µm. This very fine microcrystalline structure can only be obtained for such compositions by annealing an amorphous alloy and gives the alloy both mechanical strengths and high ductilities.
Le tableau Il donne les distances interéticulaires et les angles 6 de diffraction X (radiation K a du Cu) relatifs à la phase hxagonale rencontrée après trempe vers 200°C dans un échantillon initialement amorphe de l'alliage Al70Si15Ni15 (a = 0,6611 nm, c = 0,3780 nm).Table II gives the intereticular distances and the angles of X diffraction (radiation K a of Cu) relative to the hexagonal phase encountered after quenching around 200 ° C. in an initially amorphous sample of the alloy Al 70 Si 15 Ni 15 (a = 0.6611 nm, c = 0.3780 nm).
Nous avons élaboré 20 kg de rubans Al70Ni15Si15 par trempe sur roue. Ces rubans ont été finement broyés et la poudre ainsi obtenue a été comprimée à chaud. Le lopin de compression à chaud a été filé à 450°C avec un rapport de filage de 16:1. La barre filée a été caractérisée par traction à 20°C, à 350°C, à 450°C et à 500°C. Tous les essais de traction à chaud ont été réalisés après maintien de 10 heures à 350°C. Les résultats obtenus sont réunis dans le tableau III. Jusqu'à 350°C le matériau est très fragile et l'on observe des ruptures prématurées sur des défauts structuraux. Cependant, le niveau de charge de rupture à 350°C reste très élevé. A 450°C et 500°C le comportement est totalement différent avec des allongements élevés indicatifs d'un comportement très duètile.We produced 20 kg of Al 70 Ni 15 Si 15 ribbons by quenching on a wheel. These ribbons were finely ground and the powder thus obtained was hot pressed. The hot compression block was spun at 450 ° C with a spinning ratio of 1 6: 1. The extruded bar was characterized by traction at 20 ° C, 350 ° C, 450 ° C and 500 ° C. All of the hot tensile tests were carried out after maintaining for 10 hours at 350 ° C. The results obtained are collated in Table III. Up to 350 ° C the material is very fragile and premature ruptures on structural defects are observed. However, the level of breaking load at 350 ° C. remains very high. At 450 ° C and 500 ° C the behavior is totally different with high elongations indicative of very duetile behavior.
L'alliage Al70Ni15Si15 a été élaboré par trempe sur roue et broyé. La poudre obtenue a été projetée au moyen d'un plasma atmosphérique sur un substrat en alliage A-S5U3, ce qui conduit à une vitesse de solidification voisine de 104 K/sec. Le dépôt obtenu est à 75 % amorphe d'après un étalonnage semi-quantitatif aux rayons X (voir figure 6). La microdureté du dépôt est de 500 Vickers. Le comportement de ce dépôt à l'abrasion comparativement à celle d'un alliage A-S17U4G non revêtu, connu pour sa résistance à l'abrasion, a été étudié sur abrasimètre TABER dans les conditions suivantes :
- -meule type C5 17
- -charge appliquée : 1250 g,
avec mesure des pertes de poids au
- - grinding wheel type C5 17
- -load applied: 1250 g,
with measurement of weight losses after 300, 500, 1000, 2000 and 4000 cycles.
Les résultats obtenus sont reportés au Tableau IV et représentés graphiquement sur la figure 7.The results obtained are reported in Table IV and represented graphically in FIG. 7.
On constate que l'alliage essentiellement amorphe selon l'invention présente donc un très bon comportement au frottement et à l'abrasion.
Claims (7)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT86420062T ATE35155T1 (en) | 1985-02-27 | 1986-02-26 | AMORPHOUS ALUMINUM-BASED ALLOYS WITH NICKEL AND SILICON AS ADDITIONAL ELEMENTS AND PROCESS FOR THEIR PRODUCTION. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8503318 | 1985-02-27 | ||
FR8503318A FR2577941B1 (en) | 1985-02-27 | 1985-02-27 | AMORPHOUS AL-BASED ALLOYS CONTAINING ESSENTIALLY NI AND / OR FE AND SI AND PROCESS FOR OBTAINING SAME |
Publications (2)
Publication Number | Publication Date |
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EP0196984A1 true EP0196984A1 (en) | 1986-10-08 |
EP0196984B1 EP0196984B1 (en) | 1988-06-15 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86420062A Expired EP0196984B1 (en) | 1985-02-27 | 1986-02-26 | Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture |
Country Status (8)
Country | Link |
---|---|
US (1) | US4731133A (en) |
EP (1) | EP0196984B1 (en) |
JP (1) | JPS61210148A (en) |
AT (1) | ATE35155T1 (en) |
DE (1) | DE3660312D1 (en) |
DK (1) | DK164289C (en) |
FR (1) | FR2577941B1 (en) |
NO (1) | NO167592C (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0561204A2 (en) * | 1992-03-04 | 1993-09-22 | Toyota Jidosha Kabushiki Kaisha | Heat-resistant aluminum alloy powder, heat-resistant aluminum alloy and heat- and wear-resistant aluminum alloy-based composite material |
EP0566098A2 (en) * | 1992-04-16 | 1993-10-20 | Toyota Jidosha Kabushiki Kaisha | Heat resistant aluminum alloy powder, heat resistant aluminum alloy and heat and wear resistant aluminum alloy-based composite material |
US5409661A (en) * | 1991-10-22 | 1995-04-25 | Toyota Jidosha Kabushiki Kaisha | Aluminum alloy |
US5614036A (en) * | 1992-12-03 | 1997-03-25 | Toyota Jidosha Kabushiki Kaisha | High heat resisting and high abrasion resisting aluminum alloy |
US7136547B2 (en) | 2001-03-30 | 2006-11-14 | Gsi Group Corporation | Method and apparatus for beam deflection |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6237335A (en) * | 1985-08-09 | 1987-02-18 | Yoshida Kogyo Kk <Ykk> | Aluminum alloy having high corrosion resistance and strength |
JPH0651896B2 (en) * | 1985-07-29 | 1994-07-06 | アルミニウム粉末冶金技術研究組合 | Heat and wear resistant aluminum alloy |
JPS63153237A (en) * | 1986-08-27 | 1988-06-25 | Masumoto Takeshi | Aluminum-base alloy |
JPS6487785A (en) * | 1987-09-29 | 1989-03-31 | Showa Aluminum Corp | Production of aluminum alloy material having excellent surface hardness and wear resistance |
JP2538692B2 (en) * | 1990-03-06 | 1996-09-25 | ワイケイケイ株式会社 | High strength, heat resistant aluminum base alloy |
JPH0441602A (en) * | 1990-06-05 | 1992-02-12 | Honda Motor Co Ltd | Manufacture of high strength structural member and raw material powder aggregate |
US5432011A (en) * | 1991-01-18 | 1995-07-11 | Centre National De La Recherche Scientifique | Aluminum alloys, substrates coated with these alloys and their applications |
FR2685349B1 (en) * | 1991-12-20 | 1994-03-25 | Centre Nal Recherc Scientifique | THERMAL PROTECTION ELEMENT CONSISTING OF A QUASI-CRYSTALLINE ALUMINUM ALLOY. |
US6699336B2 (en) * | 2000-01-13 | 2004-03-02 | 3M Innovative Properties Company | Amorphous electrode compositions |
US6664004B2 (en) * | 2000-01-13 | 2003-12-16 | 3M Innovative Properties Company | Electrode compositions having improved cycling behavior |
US10294552B2 (en) * | 2016-01-27 | 2019-05-21 | GM Global Technology Operations LLC | Rapidly solidified high-temperature aluminum iron silicon alloys |
US10260131B2 (en) | 2016-08-09 | 2019-04-16 | GM Global Technology Operations LLC | Forming high-strength, lightweight alloys |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1599990A (en) * | 1967-12-30 | 1970-07-20 | ||
US4347076A (en) * | 1980-10-03 | 1982-08-31 | Marko Materials, Inc. | Aluminum-transition metal alloys made using rapidly solidified powers and method |
EP0100287A1 (en) * | 1982-07-06 | 1984-02-08 | CNRS, Centre National de la Recherche Scientifique | Amorphous or microcrystalline alloys based on aluminium |
-
1985
- 1985-02-27 FR FR8503318A patent/FR2577941B1/en not_active Expired - Fee Related
-
1986
- 1986-02-13 US US06/829,061 patent/US4731133A/en not_active Expired - Fee Related
- 1986-02-24 JP JP61038958A patent/JPS61210148A/en active Pending
- 1986-02-25 DK DK086086A patent/DK164289C/en active
- 1986-02-26 AT AT86420062T patent/ATE35155T1/en not_active IP Right Cessation
- 1986-02-26 DE DE8686420062T patent/DE3660312D1/en not_active Expired
- 1986-02-26 NO NO860714A patent/NO167592C/en unknown
- 1986-02-26 EP EP86420062A patent/EP0196984B1/en not_active Expired
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1599990A (en) * | 1967-12-30 | 1970-07-20 | ||
US4347076A (en) * | 1980-10-03 | 1982-08-31 | Marko Materials, Inc. | Aluminum-transition metal alloys made using rapidly solidified powers and method |
EP0100287A1 (en) * | 1982-07-06 | 1984-02-08 | CNRS, Centre National de la Recherche Scientifique | Amorphous or microcrystalline alloys based on aluminium |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5409661A (en) * | 1991-10-22 | 1995-04-25 | Toyota Jidosha Kabushiki Kaisha | Aluminum alloy |
EP0561204A2 (en) * | 1992-03-04 | 1993-09-22 | Toyota Jidosha Kabushiki Kaisha | Heat-resistant aluminum alloy powder, heat-resistant aluminum alloy and heat- and wear-resistant aluminum alloy-based composite material |
EP0561204A3 (en) * | 1992-03-04 | 1993-11-24 | Toyota Motor Co Ltd | Heat-resistant aluminum alloy powder, heat-resistant aluminum alloy and heat- and wear-resistant aluminum alloy-based composite material |
EP0566098A2 (en) * | 1992-04-16 | 1993-10-20 | Toyota Jidosha Kabushiki Kaisha | Heat resistant aluminum alloy powder, heat resistant aluminum alloy and heat and wear resistant aluminum alloy-based composite material |
EP0566098A3 (en) * | 1992-04-16 | 1993-11-24 | Toyota Motor Co Ltd | Heat resistant aluminum alloy powder, heat resistant aluminum alloy and heat and wear resistant aluminum alloy-based composite material |
US5464463A (en) * | 1992-04-16 | 1995-11-07 | Toyota Jidosha Kabushiki Kaisha | Heat resistant aluminum alloy powder heat resistant aluminum alloy and heat and wear resistant aluminum alloy-based composite material |
US5614036A (en) * | 1992-12-03 | 1997-03-25 | Toyota Jidosha Kabushiki Kaisha | High heat resisting and high abrasion resisting aluminum alloy |
US7136547B2 (en) | 2001-03-30 | 2006-11-14 | Gsi Group Corporation | Method and apparatus for beam deflection |
Also Published As
Publication number | Publication date |
---|---|
NO167592C (en) | 1991-11-20 |
FR2577941B1 (en) | 1991-02-08 |
DK164289B (en) | 1992-06-01 |
EP0196984B1 (en) | 1988-06-15 |
DK164289C (en) | 1992-12-21 |
DE3660312D1 (en) | 1988-07-21 |
ATE35155T1 (en) | 1988-07-15 |
DK86086D0 (en) | 1986-02-25 |
FR2577941A1 (en) | 1986-08-29 |
NO860714L (en) | 1986-08-28 |
DK86086A (en) | 1986-08-28 |
US4731133A (en) | 1988-03-15 |
NO167592B (en) | 1991-08-12 |
JPS61210148A (en) | 1986-09-18 |
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