EP0375571A1 - Verfahren zur Herstellung von Aluminiumlegierungen der Serie 7000 mittels Sprühabscheidung und nichtkontinuierlich verstärkten Verbundwerkstoffen, deren Matrix aus diesen Legierungen mit hoher mechanischer Festigkeit und guter Duktilität besteht - Google Patents
Verfahren zur Herstellung von Aluminiumlegierungen der Serie 7000 mittels Sprühabscheidung und nichtkontinuierlich verstärkten Verbundwerkstoffen, deren Matrix aus diesen Legierungen mit hoher mechanischer Festigkeit und guter Duktilität besteht Download PDFInfo
- Publication number
- EP0375571A1 EP0375571A1 EP89420497A EP89420497A EP0375571A1 EP 0375571 A1 EP0375571 A1 EP 0375571A1 EP 89420497 A EP89420497 A EP 89420497A EP 89420497 A EP89420497 A EP 89420497A EP 0375571 A1 EP0375571 A1 EP 0375571A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- alloys
- alloy
- composition
- series
- spray
- 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
Links
Classifications
-
- 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
- C22C21/10—Alloys based on aluminium with zinc as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/053—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with zinc as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
Definitions
- the invention relates to a process for obtaining an Al alloy of the 7000 series (Al-Zn-Mg-Cu) with high mechanical strength and good ductility by "spray-deposition" (spray deposition). More specifically, the method aims to obtain Al alloys which have in the treated state (T6) a breaking load ⁇ 800 MPa with an elongation, at least in the long direction, greater than or equal to 5%.
- the invention also relates to obtaining composite materials with very high strength, high rigidity and good ductility having as matrix the 7000 alloys described above with a particulate reinforcement of ceramics and obtained directly by "spray-deposition".
- spray-deposition is meant a process in which the metal is melted, atomized by a jet of gas at high pressure in the form of fine liquid droplets which are then directed and agglomerated on a substrate so as to form a massive and coherent deposit, containing low closed porosity.
- This deposit can be in the form of billets, tubes or plates whose geometry is controlled.
- a technique of this type is known as “Spray Deposition” by the Anglo-Saxons and is also called “OSPREY process”.
- the volume fraction of precipitates at the base of the structural hardening of the alloy (essentially of the type ⁇ -Mg Zn2 or ⁇ ′ - (Mg, Zn, Al, Cu)) becomes insufficient and it is no longer possible to obtain the high levels of mechanical characteristics (such as breaking load ⁇ 800 MPa) which are the objective of the present invention.
- the volume fraction of the second phase is too high and leads to a brittle material, with very low elongations at break, which prohibits its industrial use.
- the copper and magnesium contents must be in proportions close to the stoichiometry of the hardening precipitates.
- Mg ⁇ 2% or Cu ⁇ 0.5% the nature and the volume fraction of the precipitates formed are insufficient to achieve the targeted mechanical characteristics.
- Mg is ⁇ 4% or Cu ⁇ 2.0%, these elements are present in excess in the alloy and weaken it considerably.
- the preferred composition is: Zn from 8.7 to 13.7% 2.2 to 3.8% mg Cu from 0.6 to 1.6% at least one of the following 3 elements: Zr from 0.05 to 0.5% Mn from 0.05 to 0.8% Cr from 0.05 to 0.5% with Zr + Mn + Cr ⁇ 1.2% Fe up to 0.3% If up to 0.2% other (impurities) ⁇ 0.05% each ⁇ 0.15% total remains Al.
- the content of main elements preferably obeys the following relationship, 5.5 ⁇ Mg + Cu + Zn 6 ⁇ 6.5
- the hot transformation of the solid alloy obtained by spray-deposition generally takes place between 300 and 450 ° C, preferably by spinning, forging or rolling, in one or more successive operations; these operations may possibly be combined, for example spinning + rolling or spinning + forging / stamping.
- the hot transformation operations can be supplemented by cold operations such as rolling, drawing, etc.
- the solution is carried out between 440 and 520 ° C, between 2 and 8 hours depending on the size of the products; quenching is followed by tempering between 2 and 25 h between 90 and 150 ° C in one or more stages, the longest times generally being associated with the lowest temperatures (and vice-versa).
- the product obtained by a spray-deposition process can optionally be homogenized before hot transformation between 450 and 520 ° C for 2 to 50 hours in one or more stages.
- the invention also consists, using the alloys and the method described above, in obtaining composite materials with very high resistance (Rm ⁇ 800 MPa), high Young modulus (E ⁇ 80 GPa), with acceptable ductility by users (A ⁇ 3%), as well as good resistance to wear and friction.
- These materials are characterized by an alloy matrix of the 7xxx series of composition indicated above and a dispersion of ceramic particles of SiC, Al2O3 or B4C type (these examples not being limiting) and are obtained directly by the spray-deposition technique.
- the blanks are then hot-spun at 400 ° C in a press whose container has a diameter of 143 mm in the form of flats of section 50 x 22 mm, ie a spinning ratio of 14.6.
- the flats thus obtained are then dissolved at the temperature indicated in Table 1 for 2 h, quenched in cold water and then returned for 24 h at 120 ° C.
- the mechanical tensile characteristics in the long direction, average of 3 tests, are reported in Table 2 (Ro, 2: elastic limit at 0.2% residual deformation, Rm: breaking load; A%: elongation at break).
- alloys No. 1 to 4 according to the invention exhibit a very high level of mechanical properties, in particular with a tensile strength of ⁇ 800 MPa and a correct level of ductility, with elongations at rupture ⁇ 5% .
- Alloy 5 outside the analytical limits of the invention (Zn content too low) has much weaker mechanical characteristics than the alloys of the invention.
- Alloy 6 also outside the limits of the invention due to its too high Zn content, has a very low ductility (A%) and a plastic difference (Rm- R 0.2).
- Alloy 8 is an alloy whose composition falls within the analytical field of the alloys of the invention but which has been developed according to a powder metallurgy process described below: the alloy is melted and then atomized with nitrogen in the form powders; these are collected and sieved to 100 ⁇ m. Powders smaller than 100 ⁇ m are put in 140 mm diameter aluminum containers fitted with an orifice tube and are then degassed hot under secondary vacuum (by pumping through the tube) at a temperature of 460 ° C for 100 h. The powder containers thus degassed are sealed and then hot pressed in a blind die spinning press in a 143 mm diameter container at 450 ° C so as to reach the theoretical density of the material.
- the billets thus obtained are then machined in order to remove the material from the container and then spun under the same conditions as the billets of the previous examples.
- the product obtained is heat treated according to a similar procedure (see solution temperature in Table 1) and is characterized under the same conditions.
- the results reported in Table 1 show that the product obtained has very low ductility and plastic difference despite a relatively high level of resistance.
- An alloy of composition Al Al: 10% Zn; 3.0% Mg; 1.0% Cu; 0.1% Zr; 0.15% Cr; 0.15% Mn, rest Al was melted at 750 ° C and produced by spray-deposition in the form of 150 mm diameter billets with simultaneous coinjection of SiC particles of average size 10 ⁇ m, with a volume fraction of 15%.
- the spray-deposit conditions were as follows: - metal flow: 5.8 kg / min. - gas flow: 15 Nm3 / min. - atomizer-deposit distance: 620 mm, kept approximately constant during the test - stainless steel collector with rotating movement - oscillation of the atomizer relative to the axis of rotation of the collector
- the billets thus obtained are then peeled to ⁇ 140 mm, homogenized for 8 hours at 470 ° C, hot spun at 400 ° C in the form of flats with a section of 50 x 22 mm (spinning ratio 14.6).
- the spray-deposition process according to the invention in addition to the best compromise of mechanical characteristics obtained, has the following advantages over conventional powder metallurgy: - long and costly degassing and compaction operations are avoided - the method is safer, since there is no handling of reactive powders.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Coating By Spraying Or Casting (AREA)
- Laminated Bodies (AREA)
- Conductive Materials (AREA)
- Forging (AREA)
- Wrappers (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT89420497T ATE90976T1 (de) | 1988-12-19 | 1989-12-18 | Verfahren zur herstellung von aluminiumlegierungen der serie 7000 mittels spruehabscheidung und nichtkontinuierlich verstaerkten verbundwerkstoffen, deren matrix aus diesen legierungen mit hoher mechanischer festigkeit und guter duktilitaet besteht. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8817044A FR2640644B1 (fr) | 1988-12-19 | 1988-12-19 | Procede d'obtention par " pulverisation-depot " d'alliages d'al de la serie 7000 et de materiaux composites a renforts discontinus ayant pour matrice ces alliages a haute resistance mecanique et bonne ductilite |
FR8817044 | 1988-12-19 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0375571A1 true EP0375571A1 (de) | 1990-06-27 |
EP0375571B1 EP0375571B1 (de) | 1993-06-23 |
Family
ID=9373316
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP89420497A Expired - Lifetime EP0375571B1 (de) | 1988-12-19 | 1989-12-18 | Verfahren zur Herstellung von Aluminiumlegierungen der Serie 7000 mittels Sprühabscheidung und nichtkontinuierlich verstärkten Verbundwerkstoffen, deren Matrix aus diesen Legierungen mit hoher mechanischer Festigkeit und guter Duktilität besteht |
Country Status (14)
Country | Link |
---|---|
US (1) | US4995920A (de) |
EP (1) | EP0375571B1 (de) |
JP (1) | JPH02258935A (de) |
AT (1) | ATE90976T1 (de) |
AU (1) | AU615366B2 (de) |
BR (1) | BR8906543A (de) |
CA (1) | CA2005747C (de) |
DD (1) | DD290024A5 (de) |
DE (1) | DE68907331T2 (de) |
FR (1) | FR2640644B1 (de) |
HU (1) | HUT53681A (de) |
IL (1) | IL92727A0 (de) |
NO (1) | NO895100L (de) |
TR (1) | TR24392A (de) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994024326A1 (en) * | 1993-04-15 | 1994-10-27 | Alcan International Limited | Method of making hollow bodies |
EP0391815B1 (de) * | 1989-04-05 | 1995-01-25 | PECHINEY RECHERCHE (Groupement d'Intérêt Economique régi par l'Ordonnance du 23 Septembre 1967) | Legierung auf Aluminiumbasis mit einem hohen Modul und mit einer erhöhten mechanischen Festigkeit und Verfahren zur Herstellung |
EP0445684B1 (de) * | 1990-03-06 | 1995-09-27 | Ykk Corporation | Hochfeste, warmfeste Legierungen auf Aluminiumbasis |
WO2007011393A2 (en) * | 2004-10-26 | 2007-01-25 | Engelhard Corporation | Corrosion-resistant coating for metal substrate |
CN113481416A (zh) * | 2021-07-08 | 2021-10-08 | 中南大学 | 一种高性能Al-Zn-Mg-Cu系合金 |
CN114107768A (zh) * | 2020-08-26 | 2022-03-01 | 宝山钢铁股份有限公司 | 一种喷射铸轧高性能新型7xxx铝合金薄带的制备方法 |
Families Citing this family (22)
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---|---|---|---|---|
US5223216A (en) * | 1991-04-08 | 1993-06-29 | Allied-Signal Inc. | Toughness enhancement of al-li-cu-mg-zr alloys produced using the spray forming process |
FR2675821B1 (fr) * | 1991-04-26 | 1993-07-02 | Pechiney Recherche | Methode de preparation d'echantillons de reference pour analyse spectrographique. |
FR2838135B1 (fr) * | 2002-04-05 | 2005-01-28 | Pechiney Rhenalu | PRODUITS CORROYES EN ALLIAGES A1-Zn-Mg-Cu A TRES HAUTES CARACTERISTIQUES MECANIQUES, ET ELEMENTS DE STRUCTURE D'AERONEF |
DE102005032544B4 (de) * | 2004-07-14 | 2011-01-20 | Hitachi Powdered Metals Co., Ltd., Matsudo | Abriebsresistente gesinterte Aluminiumlegierung mit hoher Festigkeit und Herstellugsverfahren hierfür |
US20060292392A1 (en) * | 2004-10-26 | 2006-12-28 | Froning Marc J | Corrosion-resistant coating for metal substrate |
DE502005001724D1 (de) | 2005-01-19 | 2007-11-29 | Fuchs Kg Otto | Abschreckunempfindliche Aluminiumlegierung sowie Verfahren zum Herstellen eines Halbzeuges aus dieser Legierung |
US20070014277A1 (en) * | 2005-07-14 | 2007-01-18 | Yahoo! Inc. | Content router repository |
JP5059512B2 (ja) * | 2007-02-28 | 2012-10-24 | 株式会社神戸製鋼所 | 高強度、高延性Al合金およびその製造方法 |
WO2008105303A1 (ja) * | 2007-02-28 | 2008-09-04 | Kabushiki Kaisha Kobe Seiko Sho | 高強度、高延性Al合金およびその製造方法 |
CN104878262B (zh) * | 2015-05-18 | 2017-01-18 | 广东省材料与加工研究所 | 一种高强度铝合金及其制备方法 |
DE102016001500A1 (de) * | 2016-02-11 | 2017-08-17 | Airbus Defence and Space GmbH | Al-Mg-Zn-Legierung für den integralen Aufbau von ALM-Strukturen |
US11603583B2 (en) | 2016-07-05 | 2023-03-14 | NanoAL LLC | Ribbons and powders from high strength corrosion resistant aluminum alloys |
WO2020068199A2 (en) * | 2018-06-20 | 2020-04-02 | NanoAI LLC | HIGH-PERFORMANCE Al-Zn-Mg-Zr BASE ALUMINUM ALLOYS FOR WELDING AND ADDITIVE MANUFACTURING |
CN109055875A (zh) * | 2018-10-27 | 2018-12-21 | 安徽创弘精密机械有限公司 | 一种提高铝合金型材强度的热处理工艺 |
CN110527882A (zh) * | 2019-09-17 | 2019-12-03 | 苏州镁馨科技有限公司 | 一种高硬度铝合金材料 |
CN113088839A (zh) * | 2020-01-08 | 2021-07-09 | 核工业理化工程研究院 | 喷射沉积超高强铝合金的致密化处理方法、应用及其致密化预成型坯 |
CN113005376B (zh) * | 2021-02-10 | 2022-04-19 | 北京科技大学 | 一种超强高韧Al-Zn-Mg-Cu铝合金的固溶-时效热处理工艺 |
CN115961194A (zh) * | 2022-04-25 | 2023-04-14 | 江苏大学 | 锶锆钛铒四元复合微合金化的790MPa超高强度高塑性耐晶间腐蚀铝合金及制备方法 |
CN116121606A (zh) * | 2022-04-25 | 2023-05-16 | 江苏大学 | 锶锆钛钇镧五元复合微合金化800MPa强度级铝合金及其制备方法 |
CN115961193A (zh) * | 2022-04-25 | 2023-04-14 | 江苏大学 | 锶锆钛铒镧五元复合微合金化的790MPa超高强度超耐晶间腐蚀铝合金及制备方法 |
CN115961158A (zh) * | 2022-04-25 | 2023-04-14 | 江苏大学 | 锶锆钛钇铈五元复合微合金化的780MPa超高强度超耐晶间腐蚀铝合金及制备方法 |
CN116121607A (zh) * | 2022-04-25 | 2023-05-16 | 江苏大学 | 锶锆钛镧四元复合微合金化的740-780MPa超高强高塑性耐腐蚀铝合金及制备方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3563814A (en) * | 1968-04-08 | 1971-02-16 | Aluminum Co Of America | Corrosion-resistant aluminum-copper-magnesium-zinc powder metallurgy alloys |
EP0020282A1 (de) * | 1979-06-01 | 1980-12-10 | Societe Metallurgique De Gerzat | Verfahren zur Herstellung von Hohlkörpern aus einer Aluminiumlegierung und so erhaltene Produkte |
EP0105595A2 (de) * | 1982-09-03 | 1984-04-18 | Alcan International Limited | Aluminiumlegierungen |
EP0198606A1 (de) * | 1985-03-25 | 1986-10-22 | United Kingdom Atomic Energy Authority | Herstellung eines metallischen Produkts |
-
1988
- 1988-12-19 FR FR8817044A patent/FR2640644B1/fr not_active Expired - Fee Related
-
1989
- 1989-12-14 HU HU896605A patent/HUT53681A/hu unknown
- 1989-12-14 US US07/450,525 patent/US4995920A/en not_active Expired - Fee Related
- 1989-12-15 DD DD89335750A patent/DD290024A5/de not_active IP Right Cessation
- 1989-12-15 IL IL92727A patent/IL92727A0/xx unknown
- 1989-12-18 BR BR898906543A patent/BR8906543A/pt unknown
- 1989-12-18 NO NO89895100A patent/NO895100L/no unknown
- 1989-12-18 AT AT89420497T patent/ATE90976T1/de not_active IP Right Cessation
- 1989-12-18 AU AU46816/89A patent/AU615366B2/en not_active Ceased
- 1989-12-18 EP EP89420497A patent/EP0375571B1/de not_active Expired - Lifetime
- 1989-12-18 DE DE89420497T patent/DE68907331T2/de not_active Expired - Lifetime
- 1989-12-18 CA CA002005747A patent/CA2005747C/fr not_active Expired - Fee Related
- 1989-12-19 JP JP1329365A patent/JPH02258935A/ja active Pending
-
1990
- 1990-01-02 TR TR90/0007A patent/TR24392A/xx unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3563814A (en) * | 1968-04-08 | 1971-02-16 | Aluminum Co Of America | Corrosion-resistant aluminum-copper-magnesium-zinc powder metallurgy alloys |
EP0020282A1 (de) * | 1979-06-01 | 1980-12-10 | Societe Metallurgique De Gerzat | Verfahren zur Herstellung von Hohlkörpern aus einer Aluminiumlegierung und so erhaltene Produkte |
EP0105595A2 (de) * | 1982-09-03 | 1984-04-18 | Alcan International Limited | Aluminiumlegierungen |
EP0198606A1 (de) * | 1985-03-25 | 1986-10-22 | United Kingdom Atomic Energy Authority | Herstellung eines metallischen Produkts |
Non-Patent Citations (3)
Title |
---|
METALLURGICAL TRANSACTIONS, vol. 1, no. 1, janvier 1970, pages 191-197; T.F. BOWER et al.: "Development of high strength wrought aluminium-base alloys" * |
POWDER METALLURGY, vol. 28, no. 2, pages 72-78, A.R.E. SINGER et al.: "Metal matrix composites produced by spray codeposition" * |
W. HUFNAGEL: "Aluminium taschenbuch", edition 14, Aluminium Verlag Düsseldorf, DE, 1983, pages 1012-1018 * |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0391815B1 (de) * | 1989-04-05 | 1995-01-25 | PECHINEY RECHERCHE (Groupement d'Intérêt Economique régi par l'Ordonnance du 23 Septembre 1967) | Legierung auf Aluminiumbasis mit einem hohen Modul und mit einer erhöhten mechanischen Festigkeit und Verfahren zur Herstellung |
EP0445684B1 (de) * | 1990-03-06 | 1995-09-27 | Ykk Corporation | Hochfeste, warmfeste Legierungen auf Aluminiumbasis |
WO1994024326A1 (en) * | 1993-04-15 | 1994-10-27 | Alcan International Limited | Method of making hollow bodies |
US5932037A (en) * | 1993-04-15 | 1999-08-03 | Luxfer Group Limited | Method of making hollow bodies |
WO2007011393A2 (en) * | 2004-10-26 | 2007-01-25 | Engelhard Corporation | Corrosion-resistant coating for metal substrate |
WO2007011393A3 (en) * | 2004-10-26 | 2007-08-16 | Engelhard Corp | Corrosion-resistant coating for metal substrate |
CN114107768A (zh) * | 2020-08-26 | 2022-03-01 | 宝山钢铁股份有限公司 | 一种喷射铸轧高性能新型7xxx铝合金薄带的制备方法 |
CN113481416A (zh) * | 2021-07-08 | 2021-10-08 | 中南大学 | 一种高性能Al-Zn-Mg-Cu系合金 |
Also Published As
Publication number | Publication date |
---|---|
BR8906543A (pt) | 1990-09-04 |
IL92727A0 (en) | 1990-09-17 |
NO895100L (no) | 1990-06-20 |
EP0375571B1 (de) | 1993-06-23 |
NO895100D0 (no) | 1989-12-18 |
CA2005747C (fr) | 1996-04-09 |
DE68907331T2 (de) | 1993-10-21 |
TR24392A (tr) | 1991-09-01 |
US4995920A (en) | 1991-02-26 |
AU615366B2 (en) | 1991-09-26 |
DE68907331D1 (de) | 1993-07-29 |
AU4681689A (en) | 1990-06-21 |
FR2640644B1 (fr) | 1991-02-01 |
ATE90976T1 (de) | 1993-07-15 |
DD290024A5 (de) | 1991-05-16 |
FR2640644A1 (fr) | 1990-06-22 |
CA2005747A1 (fr) | 1990-06-19 |
HUT53681A (en) | 1990-11-28 |
JPH02258935A (ja) | 1990-10-19 |
HU896605D0 (en) | 1990-02-28 |
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