EP0540405B1 - Verfahren zur Herstellung von magnetischen Stahlbändern durch Direktgiessen - Google Patents
Verfahren zur Herstellung von magnetischen Stahlbändern durch Direktgiessen Download PDFInfo
- Publication number
- EP0540405B1 EP0540405B1 EP92402903A EP92402903A EP0540405B1 EP 0540405 B1 EP0540405 B1 EP 0540405B1 EP 92402903 A EP92402903 A EP 92402903A EP 92402903 A EP92402903 A EP 92402903A EP 0540405 B1 EP0540405 B1 EP 0540405B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- strip
- process according
- skin
- less
- cylinder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular fabrication or treatment of ingot or slab
- C21D8/1211—Rapid solidification; Thin strip casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
- C21D8/1233—Cold rolling
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1266—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest between cold rolling steps
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1272—Final recrystallisation annealing
Definitions
- the present invention relates to a method for producing a magnetic grain oriented steel strip having a thickness of less than 5 mm and containing in composition by weight more than 2% of silicon, less than 0.1% of carbon, inhibiting elements. secondary recrystallization, the rest being iron, by direct casting on a cylinder or between two cylinders to obtain it.
- Oriented grain magnetic sheets are used for the manufacture of large size magnetic circuits, transformers and rotating machines.
- the crystallographic direction ⁇ 001> which is the direction of easy magnetization, must be parallel to the rolling direction.
- the continuously cast slabs are hot rolled on a belt train and seeds of GOSS orientation ⁇ 110 ⁇ ⁇ 001> according to MILLER crystallographic notation are generated during this process. rolling operation.
- inhibitors such as MnS, A1N, BN and / or Sn and Sb which are partially precipitated or segregated in the hot rolled strip or precipitate during subsequent heat treatments (annealing of the hot rolled strip and / or intermediate annealing between two rolling cold). If the previous thermal cycles are adequate, the dimensions of a quantity sufficient precipitates are less than 100 nanometers after decarburization.
- the final static annealing in coils allows the selective growth of GOSS germs inherited from hot rolling thanks to the inhibition, by the precipitates, of the normal growth of grains not having the desired orientation. This is the phenomenon known as secondary recrystallization, the primary recrystallization taking place during the decarburization operation.
- a new process for directly obtaining a thin strip with a thickness of less than 5mm by pouring liquid metal between two cylinders or on a cylinder eliminates hot rolling so that the germs of GOSS can no longer be generated by hot rolling as in conventional processes. It is therefore essential to determine new casting conditions which favor the existence of GOSS germs in the thin strip in the raw casting state.
- the strip in the raw casting state, which has undergone recrystallization after solidification is isotropic, that is to say of random texture, the grains having no orientation preferential. Secondary recrystallization is obtained, after a cold reduction rate greater than 80%, during a secondary recrystallization annealing.
- the objective of the invention is to propose a process making it possible to obtain GOSS germs in a thin strip without the need to provide for a specific secondary heat treatment.
- the subject of the invention is a process for producing a magnetic steel strip with a thickness of less than 5 mm, containing in its composition by weight more than 2% of silicon, less than 0.1% of carbon, and elements which inhibit secondary recrystallization in suitable quantity, the rest being iron, this preparation being carried out by direct casting on a cylinder or between two cylinders, characterized in that it causes the formation of grains oriented ⁇ 110 ⁇ ⁇ 001> in skin , on the surface of at least one quenching zone, by subjecting the steel to brutal cooling by bringing the steel into contact with the or each cylinder, the surface temperature of which is less than 400 ° C.
- the invention also relates to an oriented grain sheet obtained from a strip produced by the process and which is characterized in that it comprises a columnar structure in the quenching zone and a non-columnar basalt structure comprising grains of the GOSS type. in skin.
- Figs. 2A and 2B show in section two strip structures at the outlet of the ingot mold, corresponding respectively to a speed of cylinders allowing the casting of a strip comprising a molten central zone at the outlet of the ingot mold (2A), and at a lower speed allowing the casting of a strip without liquid central zone at the outlet of the mold (2B).
- the control of the solidification conditions makes it possible to obtain GOSS seeds in a thin strip obtained by direct casting in the case of natural cooling, that is to say without using a specific secondary cooling involving, for example, a spraying of water.
- a possible secondary cooling can take place but it is not then intended to solve a metallurgical problem related to the structure. It can for example be imposed by technological constraints of winding or by the concern of avoiding a surface oxidation, and can be carried out for example by neutral gas sweeping.
- the seeds of GOSS are created in the mold by contact of the cast metal with the cylinders by optimizing the heat exchange conditions between the liquid metal and the surface of the cylinders and these germs are preserved. , under the center distance, and at the outlet of the mold, without the aid of a specific secondary cooling system, by controlling a specific parameter of the continuous casting process, for example the casting speed.
- the casting devices between two rolls are not equipped with additional cooling systems, the cooling of the solidified strip taking place in ambient air.
- Fig. 1 shows the temperature of the surface of the strip in contact with the cylinder during the passage of the metal between the two cylinders of the mold in continuous casting and the cooling cycle of the skin of the band at the outlet of the mold.
- the core having a higher temperature than that of the quenching zone raises the temperature of said skin (zone II).
- zone III the skin is subjected to natural cooling with ambient air which does not require the use of an accelerated cooling device such as by spraying with water.
- Curve C1 corresponds to a casting speed V1 and curve C2 to a casting speed V2> V1.
- Figs. 2A and 2B are two diagrams representing two strip structures at the outlet of the cylinders 5 and 6, comprising on the one hand a liquid central zone 7 between two quenching zones 8 and 9 (2A) and on the other hand two zones of quenching 8 and 9 juxtaposed, the central zone 7 being solidified at the outlet of the mold (2B).
- the observation of the microstructure of the Fe-Si band in the raw state of casting between two cylinders was carried out on samples so as to reveal germs of GOSS.
- the polished samples were subjected to a first attack with dilute nitric acid to reveal the grain boundaries, then to a second attack using a reagent containing hydrofluoric acid and hydrogen peroxide.
- the corrosion figures thus obtained were used for the determination of the crystal orientations of the grains and the location of the GOSS grains. It is noted that the germs of GOSS are located in the extreme skin, on the surface of the quenching zone in contact with the surface of the cylinder. It is the part solidified according to a non-columnar basaltic mode. To have GOSS grains at room temperature in the raw casting products, generate their formation during the first contact with the surface of the cylinder and preserve them by avoiding the enlargement of the adjacent columnar grains and by promoting their growth before the strip loses contact with the cylinders at the outlet of the mold.
- the metal on the strip surface undergoes rapid cooling and at the outlet of the mold the skin is subjected to heating by the core containing, if necessary, more or less liquid steel.
- the minimum temperature T min reached by the skin at the outlet of the ingot mold is less than 1400 ° C.
- the speed of natural cooling of the strip substantially equal in skin and at heart is not greater than 100 ° C / s.
- the originality of the present invention lies in the demonstration of the creation of GOSS germs in the mold, during the first contact of the liquid with the surface of the cylinder.
- Table 3 gives the experimental conditions and the structural characteristics of the strip cast between two cylinders.
- Table 4 describes the different stages of transformation of the pickled strip. Table 4 - Reduction rate of the first cold rolling 79% - Intermediate annealing 980 ° C, 1 min 30 - Reduction rate of the second cold rolling 55% - Decarburization annealing Mgo coating 870 ° C, 3 min - High temperature annealing 1200 ° C, 8 p.m.
- the quantity and the size of the manganese and copper sulphides resulting from the cooling of the strip with calm ambient air are compatible with the existence of a satisfactory inhibiting power.
- numerous precipitates identified by transmission electron microscopy have a spherical shape of approximately 10 to 100 nm in diameter.
- the inhibiting power can be reinforced by adding inhibitors, to the magnesia which is used as an annealing separator to avoid sticking of the turns of the coil during the secondary recrystallization annealing.
- the invention is applicable to processes for the direct casting of thin strips between two rolls and on a roll with a view to obtaining oriented grain sheets of conventional permeability or of high permeability. It is applicable whatever the mode of inhibition (sulphides, selenides, nitrides, segregated elements) of the normal growth of the primary recrystallization grains favoring the selective growth of the GOSS grains and whatever the downstream treatment of the band obtained by direct casting of liquid metal on a cylinder or between two cylinders.
- This downstream treatment can comprise a single cold rolling with a high reduction rate (greater than 80%) to obtain a high performance sheet or consist of a treatment classic with two or more cold rolling with intermediate annealing (s).
- the strip in the raw casting state may be annealed before cold rolling, in particular with a view to optimizing the size of the inhibitors.
- Cold rolling is followed by online processing, primary recrystallization and decarburization.
- the final annealing of the coils after coating with a milk of magnesia to avoid sticking of the turns, in a static oven promotes the phenomenon of secondary recrystallization which leads to the selective formation of the orientation grains ⁇ 110 ⁇ ⁇ 001>.
- the conditions for obtaining the strip between two cylinders can be adapted in the case of casting on a cylinder or by lateral supply of a cylinder with liquid metal.
- the ⁇ 110 ⁇ ⁇ 001> orientation grains are obtained under the same conditions, the pressure applied per millimeter of band width being zero.
- the GOSS grains are then only present on the face of the strip in contact with the cylinder.
- Table 5 gives an example of the number of GOSS grains per cm of skin and the percentage of GOSS grain on the single face in contact with the cylinder as a function of the experimental conditions for casting on a single cylinder.
- Table 5 Cylinder surface temperature (° C) 280 Casting speed (m / mm) 30 Strip thickness (mm) 1.38 Percentage of central area 0 % carbon of solidified metal 0.016 % of GOSS grains on the surface 5.8
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electromagnetism (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Continuous Casting (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Treatment Of Steel In Its Molten State (AREA)
- Soft Magnetic Materials (AREA)
- Control And Safety Of Cranes (AREA)
- Coating With Molten Metal (AREA)
Claims (14)
- Verfahren zur Herstellung eines magnetischen Stahlbandes mit einer Dicke von weniger als 5 mm, welches auf das Gewicht bezogen mehr als 2 % Silicium, weniger als 0,1 % Kohlenstoff, die sekundäre Rekristallisation verhindernde Elemente in geeigneter Menge und Eisen als Rest enthält, welche Herstellung durch Direktgießen auf einen Zylinder oder zwischen zwei Zylindern erfolgt, dadurch gekennzeichnet, daß man an der Oberfläche mindestens einer Abschreckzone die Bildung von in der Haut {110} <001>-orientierten Körnern verursacht, indem man den Stahl einer brutalen Abkühlung unterwirft durch Inkontaktbringen mit dem oder jedem Zylinder, dessen Oberflächentemperatur bei weniger als 400°C gehalten wird.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man das Band zwischen zwei auf eine Temperatur von weniger als 400°C abgekühlte Zylinder gießt und zwischen den Zylindern einen Druck von weniger als 500 kgf/mm Breite des Bandes ausübt.
- Verfahren nach irgendeinem der Ansprüche 1 und 2, dadurch gekennzeichnet, daß die Oberflächentemperatur des oder jedes Zylinders weniger als 250°C beträgt.
- Verfahren nach irgendeinem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß der Wärmeaustauschkoeffizient an der Grenzfläche Zylinder/verfestigte Haut oberhalb 0,10 cal/cm2·s·°C liegt.
- Verfahren nach irgendeinem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Haut des Bandes, die Oberfläche der Abschreckzone, gemäß einem Nicht-Säulen-Basalt-Modus verfestigt wird.
- Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Dicke der flüssigen Metallschicht im Kern des Bandes am Ausgang der Kokille weniger als 30 % der Gesamtdicke des Bandes ausmacht.
- Verfahren nach irgendeinem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß der Kohlenstoffgehalt des verfestigten Bandes oberhalb 0,01 % liegt.
- Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die durch die verfestigte Haut am Austritt der Kokille erreichte minimale Temperatur weniger als 1400°C beträgt.
- Verfahren nach irgendeinem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß die natürliche Abkühlgeschwindigkeit des verfestigten Bandes unterhalb 100°C/s liegt.
- Verfahren nach irgendeinem der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß das Band zusätzlich mindestens einem Kaltwalzvorgang, einer Wärmebehandlung zur Decarburierung und primären Rekristallisation und einer abschließenden Anlaßbehandlung zur sekundären Rekristallisation unterworfen wird.
- Verfahren nach Anspruch 10, dadurch gekennzeichnet, daß das Band nach dem oder jedem Kaltwalzen einer Anlaßbehandlung unterworfen wird.
- Verfahren nach Anspruch 10, dadurch gekennzeichnet, daß das Band vor dem ersten Kaltwalzen einer Anlaßbehandlung unterworfen wird.
- Blech mit {110} <001>-orientierten Körnern erhalten aus dem nach dem Verfahren gemäß den Ansprüchen 1 bis 9 hergestellten Band, dadurch gekennzeichnet, daß es eine Säulenstruktur in der Abschreckzone und eine Nicht-Säulen-Basaltstruktur, die Körner des GOSS-Typs in der Haut aufweist, besitzt.
- Blech nach Anspruch 13, dadurch gekennzeichnet, daß es weiterhin eine zentrale Zone mit gleichgerichteter Struktur umfaßt.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9113499 | 1991-10-31 | ||
FR9113499A FR2683229B1 (fr) | 1991-10-31 | 1991-10-31 | Procede d'elaboration d'une bande d'acier magnetique par coulee directe. |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0540405A1 EP0540405A1 (de) | 1993-05-05 |
EP0540405B1 true EP0540405B1 (de) | 1997-01-22 |
Family
ID=9418534
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP92402903A Expired - Lifetime EP0540405B1 (de) | 1991-10-31 | 1992-10-26 | Verfahren zur Herstellung von magnetischen Stahlbändern durch Direktgiessen |
Country Status (16)
Country | Link |
---|---|
US (1) | US5417772A (de) |
EP (1) | EP0540405B1 (de) |
JP (1) | JP2863679B2 (de) |
AT (1) | ATE148175T1 (de) |
CZ (1) | CZ284160B6 (de) |
DE (2) | DE69216994T2 (de) |
DK (1) | DK0540405T3 (de) |
ES (1) | ES2099233T3 (de) |
FR (1) | FR2683229B1 (de) |
GR (1) | GR3023079T3 (de) |
HU (1) | HU214854B (de) |
PL (1) | PL171088B1 (de) |
RO (1) | RO114349B1 (de) |
RU (1) | RU2105074C1 (de) |
SK (1) | SK281332B6 (de) |
UA (1) | UA26031C2 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19745445C1 (de) * | 1997-10-15 | 1999-07-08 | Thyssenkrupp Stahl Ag | Verfahren zur Herstellung von kornorientiertem Elektroblech mit geringem Ummagnetisierungsverlust und hoher Polarisation |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
IT1316029B1 (it) | 2000-12-18 | 2003-03-26 | Acciai Speciali Terni Spa | Processo per la produzione di acciaio magnetico a grano orientato. |
US7059384B2 (en) * | 2001-06-15 | 2006-06-13 | National Research Council Of Canada | Apparatus and method for metal strip casting |
AU2002326892B2 (en) * | 2001-09-13 | 2007-06-21 | Ak Steel Properties, Inc. | Method of continuously casting electrical steel strip with controlled spray cooling |
AU2008100847A4 (en) * | 2007-10-12 | 2008-10-09 | Bluescope Steel Limited | Method of forming textured casting rolls with diamond engraving |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3061486A (en) * | 1957-12-30 | 1962-10-30 | Armco Steel Corp | Non-directional oriented silicon-iron |
US3115430A (en) * | 1960-09-20 | 1963-12-24 | Armco Steel Corp | Production of cube-on-edge oriented silicon iron |
JPS6017625B2 (ja) * | 1982-05-24 | 1985-05-04 | 川崎製鉄株式会社 | 双ロ−ル式急冷薄帯製造方法および装置 |
JPS6179724A (ja) * | 1984-09-28 | 1986-04-23 | Nippon Kokan Kk <Nkk> | 高珪素鉄合金の薄板製造方法 |
US5259443A (en) * | 1987-04-21 | 1993-11-09 | Nippon Yakin Kogyo Co., Ltd. | Direct production process of a length of continuous thin two-phase stainless steel strip having excellent superplasticity and surface properties |
DE8816779U1 (de) * | 1988-08-13 | 1990-08-16 | Kiekert GmbH & Co KG, 5628 Heiligenhaus | Kraftfahrzeug-Türverschlußvorrichtung |
JPH02258149A (ja) * | 1989-03-30 | 1990-10-18 | Nippon Steel Corp | 一方向性高磁束密度電磁鋼板の製造方法 |
US5049204A (en) * | 1989-03-30 | 1991-09-17 | Nippon Steel Corporation | Process for producing a grain-oriented electrical steel sheet by means of rapid quench-solidification process |
US5259439A (en) * | 1990-04-04 | 1993-11-09 | Ishikawajima-Harima Heavy Industries Company Limited | Strip casting |
-
1991
- 1991-10-31 FR FR9113499A patent/FR2683229B1/fr not_active Expired - Fee Related
-
1992
- 1992-10-26 DE DE69216994T patent/DE69216994T2/de not_active Expired - Fee Related
- 1992-10-26 DK DK92402903.6T patent/DK0540405T3/da active
- 1992-10-26 AT AT92402903T patent/ATE148175T1/de not_active IP Right Cessation
- 1992-10-26 ES ES92402903T patent/ES2099233T3/es not_active Expired - Lifetime
- 1992-10-26 EP EP92402903A patent/EP0540405B1/de not_active Expired - Lifetime
- 1992-10-28 US US07/967,439 patent/US5417772A/en not_active Expired - Lifetime
- 1992-10-28 DE DE4236359A patent/DE4236359A1/de not_active Ceased
- 1992-10-29 PL PL92296412A patent/PL171088B1/pl not_active IP Right Cessation
- 1992-10-30 SK SK3279-92A patent/SK281332B6/sk unknown
- 1992-10-30 RU RU92004372A patent/RU2105074C1/ru not_active IP Right Cessation
- 1992-10-30 HU HU9203426A patent/HU214854B/hu not_active IP Right Cessation
- 1992-10-30 RO RO92-01362A patent/RO114349B1/ro unknown
- 1992-10-30 CZ CS923279A patent/CZ284160B6/cs not_active IP Right Cessation
- 1992-11-02 JP JP4294481A patent/JP2863679B2/ja not_active Expired - Fee Related
-
1993
- 1993-06-15 UA UA93002909A patent/UA26031C2/uk unknown
-
1997
- 1997-04-08 GR GR970400747T patent/GR3023079T3/el unknown
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19745445C1 (de) * | 1997-10-15 | 1999-07-08 | Thyssenkrupp Stahl Ag | Verfahren zur Herstellung von kornorientiertem Elektroblech mit geringem Ummagnetisierungsverlust und hoher Polarisation |
Also Published As
Publication number | Publication date |
---|---|
HU9203426D0 (en) | 1993-03-01 |
RO114349B1 (ro) | 1999-03-30 |
RU2105074C1 (ru) | 1998-02-20 |
ES2099233T3 (es) | 1997-05-16 |
PL171088B1 (pl) | 1997-03-28 |
FR2683229A1 (fr) | 1993-05-07 |
JP2863679B2 (ja) | 1999-03-03 |
JPH06142851A (ja) | 1994-05-24 |
DE69216994D1 (de) | 1997-03-06 |
DE69216994T2 (de) | 1997-06-12 |
PL296412A1 (en) | 1993-07-12 |
DK0540405T3 (da) | 1997-02-10 |
DE4236359A1 (de) | 1993-05-06 |
SK327992A3 (en) | 1995-07-11 |
FR2683229B1 (fr) | 1994-02-18 |
HU214854B (hu) | 1998-06-29 |
EP0540405A1 (de) | 1993-05-05 |
HUT71567A (en) | 1995-12-28 |
ATE148175T1 (de) | 1997-02-15 |
US5417772A (en) | 1995-05-23 |
GR3023079T3 (en) | 1997-07-30 |
UA26031C2 (uk) | 1999-02-26 |
CZ327992A3 (en) | 1994-03-16 |
CZ284160B6 (cs) | 1998-09-16 |
SK281332B6 (sk) | 2001-02-12 |
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