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EP0313888B2 - Method for hardening of work pieces of steel - Google Patents
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EP0313888B2 - Method for hardening of work pieces of steel - Google Patents

Method for hardening of work pieces of steel Download PDF

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Publication number
EP0313888B2
EP0313888B2 EP88116477A EP88116477A EP0313888B2 EP 0313888 B2 EP0313888 B2 EP 0313888B2 EP 88116477 A EP88116477 A EP 88116477A EP 88116477 A EP88116477 A EP 88116477A EP 0313888 B2 EP0313888 B2 EP 0313888B2
Authority
EP
European Patent Office
Prior art keywords
cooling gas
helium
mpa
hydrogen
quenching
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
Application number
EP88116477A
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German (de)
French (fr)
Other versions
EP0313888B1 (en
EP0313888A1 (en
Inventor
Paul Dipl.-Ing. Heilmann
Friedrich Dipl.Phys.Dr. Preisser
Rolf Schuster
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ALD Vacuum Technologies GmbH
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ALD Vacuum Technologies GmbH
Priority date (The priority date 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 date listed.)
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Publication date
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Application filed by ALD Vacuum Technologies GmbH filed Critical ALD Vacuum Technologies GmbH
Priority to AT88116477T priority Critical patent/ATE65801T1/en
Publication of EP0313888A1 publication Critical patent/EP0313888A1/en
Publication of EP0313888B1 publication Critical patent/EP0313888B1/en
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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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/767—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material with forced gas circulation; Reheating thereof
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/613—Gases; Liquefied or solidified normally gaseous material
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories or equipment specially adapted for furnaces of these types
    • F27B5/16—Arrangements of air or gas supply devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories or equipment specially adapted for furnaces of these types
    • F27B5/16—Arrangements of air or gas supply devices
    • F27B2005/161—Gas inflow or outflow

Definitions

  • the invention relates to a method for hardening workpieces made of steel in a vacuum oven by heating the workpieces and then quenching in a cooling gas Overpressure and cooling gas circulation.
  • This object is achieved in that helium, hydrogen, mixtures of helium and hydrogen or mixtures of helium and / or water inert gas are used as cooling gas in that the cooling gas pressure "p" in the furnace is set to values between 1 and 4 MPa during quenching , and that the cooling gas velocity "v" is chosen so that the product p ⁇ v is between 10 and 250 m ⁇ MPa ⁇ sec -1 .
  • cooling gas Helium or helium mixtures with up to 30 vol% Hydrogen and / or inert gases.
  • the cooling gas velocity "V" refers to the outlet from the cooling gas distribution pipes.
  • the steel parts are heated in a vacuum oven customary for this purpose.
  • the furnace is advantageously flooded with the helium or hydrogen gas at the start of the heating at about 2 MPa pressure and the gas is circulated with a fan.
  • This has the advantage that the heat is transferred to the steel parts not by radiation but by convection, which results in a uniform heating of the batch and a considerable reduction in the heating time.
  • the gas is removed from the oven and further heated under vacuum. In this temperature range, the radiation heating is very effective and a protective gas for heating the batches is not necessary.
  • the furnace is flooded with cold cooling gas up to 4 MPa overpressure to cool the batch.
  • the cooling gas is circulated with the aid of a fan, cooled down via a heat exchanger after leaving the furnace interior and fed back to the batch. This circulation continues until the batch has cooled.
  • the gas velocity is adjusted with the help of the fan so that the product pv between 10 and 250 mMPa sec -1 .
  • a component with a diameter of approx. 10 mm made of the low alloy steel 100 Cr6 is heated in a vacuum furnace to the austenitizing temperature of approx. 850 ° C. After this temperature has been reached, the furnace is flooded with helium to an excess pressure of 1.6 MPa, the sample being cooled to 400 ° C. in 16 seconds at a gas velocity of 65 m.sec -1 , which corresponds to the cooling rate in an oil bath .
  • a martensitic structure with a hardness of 64 HRC is obtained.
  • the steel 100 6Cr cannot be hardened with the gas quenching processes known to date.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Heat Treatments In General, Especially Conveying And Cooling (AREA)
  • Heat Treatment Of Articles (AREA)
  • Control Of Heat Treatment Processes (AREA)
  • Furnace Details (AREA)
  • Resistance Heating (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Physical Vapour Deposition (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)
  • Muffle Furnaces And Rotary Kilns (AREA)
  • Electronic Switches (AREA)

Abstract

A process for heat treatment of metallic workpieces by heating in a vacuum furnace followed by quenching in a coolant gas under above-atmospheric pressure and with coolant-gas circulation.

Description

Die Erfindung betrifft ein Verfahren zum Härten von Werkstükken aus Stahl in einem Vakuumofen durch Aufheizen der Werkstücke und anschließendes Abschrecken in einem Kühlgas unter Überdruck und Kühlgasumwälzung.The invention relates to a method for hardening workpieces made of steel in a vacuum oven by heating the workpieces and then quenching in a cooling gas Overpressure and cooling gas circulation.

Zum Härten metallischer Werkstücke, insbesondere Werkzeuge, werden diese in einem Ofen auf die Austenitisierungstemperatur des Werkstoffs erhitzt und dann abgeschreckt. Je nach Werkstoffart und gewünschter mechanischer Eigenschaften sind zum Abschrecken Bäder aus Wasser, Öl oder geschmolzenen Salzen erforderlich. Teile aus Schnellarbeitsstählen und anderen hocheegierten Werkstoffen können auch in Inertgasen abgeschreckt werden, wenn diese kontinuierlich gekühlt und umgewälzt werden.For hardening metallic workpieces, in particular Tools, these are placed in an oven on the Austenitizing temperature of the material heated and then quenched. Depending on the type of material and desired mechanical properties are for Quench baths of water, oil, or melted Salting is required. High-speed steel parts and other highly alloyed materials can also be quenched in inert gases, if it is continuously cooled and circulated will.

In der DE-PS 28 39 807 und der DE-PS 28 44 343 werden Vakuumöfen beschrieben, in denen zum Abschrecken Kühlgase mit hoher Gasgeschwindigkeit und mit Drücken bis zu 0,6 MPa (6 bar) über die aufgehelzten Werkstückchargen und anschließend über Wärmetauscher geleitet werden. Die erforderlichen hohen Kühlgasgeschwindigkeiten erreicht man mit Hilfe von Düsen oder Ventilatoren. Höhere Abschreckgeschwindigkeiten kann man im Prinzip durch Erhöhung des Kühlgasdrucks erzielen, doch erreicht man bei den derzeit verwendeten Kühlgasen (z. B. Stickstoff, Argon) nur einen Überdruck bis zu etwa 0,6 MPa. Die Anwendung höherer Drücke wird durch die Motorleistung begrenzt, die zur Umwälzung der komprimierten Gase erforderlich ist Bei Verwendung von Stickstoff als Kühlgas mit 0,6 MPa Überdruck beträgt die erforderliche Motorenleistung bei einem Ventilator bereits über 100 kW. Motoren mit höheren Leistungen sind aber sehr voluminös, teuer und für einen Einbau in einen Vakuumofen normalerweise nicht geeignet.In DE-PS 28 39 807 and DE-PS 28 44 343 vacuum ovens are described in which Quenching cooling gases at high gas velocity and with pressures up to 0.6 MPa (6 bar) above the melted workpiece batches and then be passed through heat exchangers. The necessary high cooling gas speeds can be achieved with the help of nozzles or fans. Higher Quenching speeds can in principle by increasing the cooling gas pressure, yes can be achieved with the cooling gases currently used (e.g. nitrogen, argon) only an excess pressure up to about 0.6 MPa. The application of higher pressures will limited by the engine power required for circulation the compressed gases is required when using of nitrogen as cooling gas with 0.6 MPa overpressure is the required engine power at a fan already over 100 kW. Engines with higher performances are very voluminous, expensive and usually for installation in a vacuum oven not suitable.

Durch diese technisch bedingte Begrenzung der Kühlgasumwälzung und des Kühlgasdrucks war es bisher nicht möglich, höhere Abschreckintensitäten mit Kühlgasen zu erreichen, so daß das Abschreckverfahren mit Kühlgasen auf spezielle Werkstoffe beschränkt ist.Due to this technical limitation of It was cooling gas circulation and the cooling gas pressure previously not possible, higher quenching intensities to achieve with cooling gases, so the quenching process with cooling gases on special materials is limited.

Es war Aufgabe der vorliegenden Erfindung, ein Verfahren zum Härten von Werkstücken aus Stahl in einem Vakuumofen durch Aufheizen der Werkstücke und anschließendes Abschrecken in einem Kühlgas unter Überdruck und Kühlgasumwälzung zu entwickeln, mit dem eine höhere Abschreckintensität erzielbar ist, ohne die Motorenleistung für die Kühlgasumwälzung erhöhen zu müssen.It was an object of the present invention Process for hardening workpieces made of steel in a vacuum oven by heating the Workpieces and subsequent quenching in one Cooling gas under excess pressure and cooling gas circulation to develop with a higher Quench intensity is achievable without the engine power need to increase for the cooling gas circulation.

Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß als Kühlgas Helium, Wasserstoff, Gemische aus Helium und Wasserstoff oder Gemische aus Helium und/oder Wassernertgas verwendet werden, daß der Kühlgasdruck "p" im Ofen bei der Abschreckung auf Werte zwischen 1 und 4 MPa eingestellt wird, und daß die Kühlgasgeschwindigkeit "v" so gewählt wird, daß das Produkt p·v zwischen 10 und 250 m·MPa·sec-1 liegt.This object is achieved in that helium, hydrogen, mixtures of helium and hydrogen or mixtures of helium and / or water inert gas are used as cooling gas in that the cooling gas pressure "p" in the furnace is set to values between 1 and 4 MPa during quenching , and that the cooling gas velocity "v" is chosen so that the product p · v is between 10 and 250 m · MPa · sec -1 .

Vorzugsweise verwendet man als Kühlgas Helium oder Heliumgemische mit bis zu 30 Vol% Wasserstoff und/oder Inertgasen.Preferably used as the cooling gas Helium or helium mixtures with up to 30 vol% Hydrogen and / or inert gases.

Als günstig hat es sich erwiesen, im Ofen einen Kühlgasdruck zwischen 1,4 und 3,0 MPa einzustellen und die Kühlgasumwälzung mit einem Ventilator vorzunehmen.It has proven to be cheap to have one in the oven Set the cooling gas pressure between 1.4 and 3.0 MPa and carry out the cooling gas circulation with a fan.

Die Kühlgasgeschwindigkeit "V" bezieht sich auf den Austritt aus den Kühlgasverteilungsrohren.The cooling gas velocity "V" refers to the outlet from the cooling gas distribution pipes.

Es hat sich überraschenderweise erwiesen, daß bei Verwendung von Helium und/oder Wasserstoff bzw. deren Gemische mit bis zu 30 Vol% Inertgas, wie z. B. Stickstoff, als Kühlgas in den entsprechenden Öfen Drücke bis zu 4 MPa eingestellt werden können, ohne daß die Motorleistung der verwendeten Ventilatoren erhöht werden müssen. Dadurch wird die Kühlwirkung der Gase derart verstärkt, daß ein wesentlich breiteres Spektrum von Stählen gehärtet werden kann, auch solche Stahlsorten, die man bisher in einem Ölbad abschrecken musste. Diese Hochdruck-Gasabschreckung hat gegenüber flüssigen Abschreckmedien verfahrenstechnische und wirtschaftliche Vorteile. Außerdem ist sie umweltfreundlicher.It has surprisingly been found that when using helium and / or hydrogen or their mixtures with up to 30 vol% inert gas, such as e.g. B. nitrogen, as a cooling gas in the corresponding Furnace pressures can be set up to 4 MPa without the motor power of the fans used need to be increased. This will have the cooling effect the gases so intensified that a substantial wider range of steels can be hardened can, even those types of steel that were previously in one Oil bath had to put you off. This high pressure gas quenching compared to liquid Quenching media procedural and economic Advantages. It is also more environmentally friendly.

Bei der praktischen Ausführung dieses Verfahrens werden die Stahlteile in einem für diesen Zweck üblichen Vakuumofen aufgeheizt. Dabei flutet man den Ofen vorteilhafterweise mit dem Helium- bzw. Wasserstoffgas bereits zu Beginn der Aufheizung mit etwa 2 MPa Druck und wälzt das Gas mit einem Ventilator um. Das hat den Vorteil, daß die Wärmeübertragung auf die Stahlteile nicht durch Strahlung sondern durch Konvektion erfolgt, was ein gleichmäßiges Aufheizen der Charge und eine beträchtliche Verkürzung der Aufheizzeit zur Folge hat. Oberhalb 750°C wird das Gas aus dem Ofen entfernt und unter Vakuum weitererhitzt. In diesem Temperaturbereich ist die Strahlungserwärmung sehr wirksam und ein Schutzgas zur Erwärmung der Chargen nicht notwendig. Nach Erreichen der jeweiligen Austenitisierungtemperatur, die zwischen 800 und 1300°C liegen kann, wird zum Abkühlen der Charge der Ofen mit kaltem Kühlgas bis zu 4 MPa Überdruck geflutet. Das Kühlgas wird mit Hilfe eines Ventilators umgewälzt, nach Verlassen des Ofeninnenraums über einen Wärmetauscher abgekühlt und erneut der Charge zugeleitet. Diese Umwälzung erfolgt solange, bis die Charge abgekühlt ist. Die Gasgeschwindigkeit wird dabei mit Hilfe des Ventilators so eingestellt, daß das Produkt p·v zwischen 10 und 250 m·MPa·sec-1 liegt.In the practical implementation of this method, the steel parts are heated in a vacuum oven customary for this purpose. The furnace is advantageously flooded with the helium or hydrogen gas at the start of the heating at about 2 MPa pressure and the gas is circulated with a fan. This has the advantage that the heat is transferred to the steel parts not by radiation but by convection, which results in a uniform heating of the batch and a considerable reduction in the heating time. Above 750 ° C, the gas is removed from the oven and further heated under vacuum. In this temperature range, the radiation heating is very effective and a protective gas for heating the batches is not necessary. After reaching the respective austenitizing temperature, which can be between 800 and 1300 ° C, the furnace is flooded with cold cooling gas up to 4 MPa overpressure to cool the batch. The cooling gas is circulated with the aid of a fan, cooled down via a heat exchanger after leaving the furnace interior and fed back to the batch. This circulation continues until the batch has cooled. The gas velocity is adjusted with the help of the fan so that the product pv between 10 and 250 mMPa sec -1 .

Folgendes Beispiel soll das erfindungsgemäße Verfahren näher erläutern :
Ein Bauteil mit ca. 10 mm Durchmesser aus dem niedriglegierten Stahl 100 Cr6 wird in einem Vakuumofen auf die Austenitisierungstemperatur von ca. 850°C erwärmt. Nach Erreichen dieser Temperatur wird der Ofen mit Helium bis zu einem Überdruck von 1,6 MPa geflutet, wobei bei einer Gasgeschwindigkeit von 65 m·sec-1 in 16 sec die Probe auf 400°C heruntergekühlt war, was der Abkühlgeschwindigkeit in einem Ölbad entspricht. Man erhält einen martensitischen Gefügezustand mit einer Härte von 64 HRC. Mit den bisher bekannten Gasabschreckungsverfahren läßt sich der Stahl 100 6Cr nicht härten.The following example is intended to explain the process according to the invention in more detail:
A component with a diameter of approx. 10 mm made of the low alloy steel 100 Cr6 is heated in a vacuum furnace to the austenitizing temperature of approx. 850 ° C. After this temperature has been reached, the furnace is flooded with helium to an excess pressure of 1.6 MPa, the sample being cooled to 400 ° C. in 16 seconds at a gas velocity of 65 m.sec -1 , which corresponds to the cooling rate in an oil bath . A martensitic structure with a hardness of 64 HRC is obtained. The steel 100 6Cr cannot be hardened with the gas quenching processes known to date.

Claims (4)

  1. Process for the hardening of workpieces of steel in a vacuum furnace by heating the workpieces and then quenching them in a cooling gas under excess pressure and with cooling gas circulation, characterized in that the cooling gas used is helium, hydrogen, mixtures of helium and hydrogen or mixtures of helium and/or hydrogen with up to 30 vol.% of inert gas, in that the cooling gas pressure "p" in the furnace during quenching is set to values between 1 and 4 MPa and in that the cooling gas velocity "V" is selected in such a way that the product p . v is between 10 and 250 m . MPa . sec-1.
  2. Process according to Claim 1, characterized in that helium or helium mixtures with up to 30 vol.% of hydrogen and/or inert gases are used as cooling gas.
  3. Process according to Claim 1 and 2, characterized in that a cooling gas pressure between 1.4 and 3.0 MPa is set in the furnace during quenching.
  4. Process according to Claim 1 to 3, characterized in that the cooling gas circulation takes place with a fan.
EP88116477A 1987-10-28 1988-10-05 Method for hardening of work pieces of steel Expired - Lifetime EP0313888B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88116477T ATE65801T1 (en) 1987-10-28 1988-10-05 METHOD OF HEAT TREATMENT OF METALLIC WORKPIECES.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3736501A DE3736501C1 (en) 1987-10-28 1987-10-28 Process for the heat treatment of metallic workpieces
DE3736501 1987-10-28

Publications (3)

Publication Number Publication Date
EP0313888A1 EP0313888A1 (en) 1989-05-03
EP0313888B1 EP0313888B1 (en) 1991-07-31
EP0313888B2 true EP0313888B2 (en) 1998-06-17

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ID=6339263

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88116477A Expired - Lifetime EP0313888B2 (en) 1987-10-28 1988-10-05 Method for hardening of work pieces of steel

Country Status (28)

Country Link
US (1) US4867808A (en)
EP (1) EP0313888B2 (en)
JP (1) JP3068135B2 (en)
CN (1) CN1015066B (en)
AT (1) ATE65801T1 (en)
AU (1) AU606473B2 (en)
BG (1) BG49828A3 (en)
BR (1) BR8805492A (en)
CA (1) CA1308631C (en)
CS (1) CS274632B2 (en)
DD (1) DD283421A5 (en)
DE (2) DE3736501C1 (en)
DK (1) DK167497B1 (en)
ES (1) ES2023993T5 (en)
FI (1) FI86560C (en)
HR (1) HRP920581B1 (en)
HU (1) HU204102B (en)
IL (1) IL87762A (en)
MX (1) MX169690B (en)
NO (1) NO169244C (en)
PL (1) PL159767B1 (en)
PT (1) PT88896A (en)
RO (1) RO110067B1 (en)
RU (1) RU1813104C (en)
SI (1) SI8811937A8 (en)
UA (1) UA13002A (en)
YU (1) YU46574B (en)
ZA (1) ZA886853B (en)

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US6776854B2 (en) 2001-02-28 2004-08-17 Vacuheat Gmbh Process and apparatus for the partial thermochemical vacuum treatment of metallic workpieces

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DE4132712C2 (en) * 1991-10-01 1995-06-29 Ipsen Ind Int Gmbh Vacuum furnace for plasma carburizing metallic workpieces
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EP0803583B2 (en) * 1996-04-26 2009-12-16 Nippon Steel Corporation Primary cooling method in continuously annealing steel strips
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CN105695716A (en) * 2016-01-29 2016-06-22 柳州市安龙机械设备有限公司 Heat treatment method for hard alloy cutter

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FI884513L (en) 1989-04-29
FI86560C (en) 1992-09-10
HUT49651A (en) 1989-10-30
JP3068135B2 (en) 2000-07-24
IL87762A (en) 1993-01-31
US4867808A (en) 1989-09-19
DK596588A (en) 1989-04-29
ES2023993T5 (en) 1998-08-01
AU606473B2 (en) 1991-02-07
RU1813104C (en) 1993-04-30
PL159767B1 (en) 1993-01-29
DK167497B1 (en) 1993-11-08
UA13002A (en) 1997-02-28
DE3736501C1 (en) 1988-06-09
FI86560B (en) 1992-05-29
EP0313888B1 (en) 1991-07-31
CS711188A2 (en) 1990-10-12
PT88896A (en) 1989-09-14
FI884513A0 (en) 1988-09-30
NO884389L (en) 1989-05-02
ATE65801T1 (en) 1991-08-15
SI8811937A8 (en) 1997-06-30
CN1015066B (en) 1991-12-11
ZA886853B (en) 1989-05-30
DK596588D0 (en) 1988-10-27
PL275471A1 (en) 1989-05-02
BG49828A3 (en) 1992-02-14
NO169244B (en) 1992-02-17
EP0313888A1 (en) 1989-05-03
HRP920581B1 (en) 1997-10-31
CA1308631C (en) 1992-10-13
DE3864007D1 (en) 1991-09-05
RO110067B1 (en) 1995-09-29
IL87762A0 (en) 1989-02-28
US4867808B1 (en) 1994-02-22
DD283421A5 (en) 1990-10-10
CS274632B2 (en) 1991-09-15
HU204102B (en) 1991-11-28
ES2023993B3 (en) 1992-02-16
NO884389D0 (en) 1988-10-04
YU46574B (en) 1993-11-16
MX169690B (en) 1993-07-19
HRP920581A2 (en) 1995-02-28
JPH01149920A (en) 1989-06-13
BR8805492A (en) 1989-07-04
NO169244C (en) 1992-05-27
YU193788A (en) 1990-04-30
CN1033841A (en) 1989-07-12
AU2440488A (en) 1989-05-04

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