EP0046230B1 - Pyrotechnic fog or smoke producing charge having a casing, its composition and method for its manufacture - Google Patents

Pyrotechnic fog or smoke producing charge having a casing, its composition and method for its manufacture Download PDF

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Publication number
EP0046230B1
EP0046230B1 EP81106031A EP81106031A EP0046230B1 EP 0046230 B1 EP0046230 B1 EP 0046230B1 EP 81106031 A EP81106031 A EP 81106031A EP 81106031 A EP81106031 A EP 81106031A EP 0046230 B1 EP0046230 B1 EP 0046230B1
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EP
European Patent Office
Prior art keywords
composition
pyrotechnic charge
ignition
smoke
binder
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
Application number
EP81106031A
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German (de)
French (fr)
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EP0046230A2 (en
EP0046230A3 (en
Inventor
Manfred Weber
Friedmar Hinzmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Piepenbrock Pyrotechnik Te Goellheim Bondsre GmbH
Original Assignee
Pyrotechnische Fabrik F Feistel GmbH and Co KG
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Priority to AT81106031T priority Critical patent/ATE17167T1/en
Publication of EP0046230A2 publication Critical patent/EP0046230A2/en
Publication of EP0046230A3 publication Critical patent/EP0046230A3/en
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Publication of EP0046230B1 publication Critical patent/EP0046230B1/en
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D3/00—Generation of smoke or mist (chemical part)
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42—AMMUNITION; BLASTING
    • F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
    • F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
    • F42B12/02—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect
    • F42B12/36—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information
    • F42B12/44—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information of incendiary type
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42—AMMUNITION; BLASTING
    • F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
    • F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
    • F42B12/02—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect
    • F42B12/36—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information
    • F42B12/46—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information for dispensing gases, vapours, powders or chemically-reactive substances
    • F42B12/48—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information for dispensing gases, vapours, powders or chemically-reactive substances smoke-producing, e.g. infrared clouds
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42—AMMUNITION; BLASTING
    • F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
    • F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
    • F42B12/72—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the material
    • F42B12/76—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the material of the casing

Definitions

  • the invention relates to a pyrotechnic charge in the form of smoke or incendiary charges in the form of pressed bodies stacked in layers in a shell provided with longitudinal target breaking points and having a central recess in which an ignition charge is arranged, and methods for their production.
  • mist-producing substances or mixtures of substances and devices which fire them into or over a target area are known.
  • the mist mixtures are shaped and pressed into compacts, stacked in a metal sleeve and, if ignited, ejected from the sleeve opening, if necessary using an igniter, whereby they are distributed conically like a shot.
  • a fire set with the features of the preamble of claim 1 is known, which is provided for firing from a hand-held device.
  • the shell is designed so that it collapses mechanically over its entire length in the event of an impact.
  • a metal tube is arranged in the central recess, in which a glow plug and a disassembly set are arranged adjacent to one another, the wall of the metal tube being reinforced in the area of the glow plug.
  • a device for producing an artificial fog blanket in which the pressing bodies are stacked in a burst-proof envelope around an ignition tube.
  • This device has considerable disadvantages.
  • the space in the casing is therefore not optimally used due to the segmented pressing bodies stacked in it. Rather, there are cavities that reduce the charge density.
  • an increased amount of dust in the mist set which causes the effect of reducing material loss, arises in particular during manufacture and during transport due to abrasion at the interfaces of the pressed bodies.
  • the manufacturing outlay is also considerable, both for producing the segmented pressing bodies and for inserting them into a charge envelope using an ignition tube.
  • the individual segments are designed in such a way that they are partially destroyed into small particles by the pressure load that occurs during ignition.
  • the shell usually made of metal, from which the smoke or incendiary devices are ejected at a certain height, then falls undamaged as a part to the ground and can also cause serious injuries under unfavorable circumstances.
  • Another disadvantage of the known charges used as a mist set arises from the composition of the mist mixture. These often react acidic or develop phosphorus pentoxide, which is converted to phosphoric acid in the air, cause breathing difficulties and coughing or attack internal organs. Such disadvantages are particularly undesirable when one thinks of the use of fog loads in wine-growing areas to prevent frost or when used for training and maneuvering purposes.
  • DE-B-2451 701 describes a smoke or mist set which contains an organic chlorine donor, metal powder and / or metal oxide.
  • the known mist set contains at least one of the high molecular weight chlorine donors chloroparaffin, chlorinated polyphenylene, chlorinated polyphenoxy resin and polyester from tetrachlorophthalic acid with chlorinated polyalcohol as a binder.
  • smoke and mist sets consist of a mixture of hexachloroethane with metal powder such as zinc, aluminum, titanium, magnesium and iron.
  • Usual igniter sets for fire or smoke sets contain magnesium powder, black powder flour and a binding agent as main components. They have the disadvantage that they do not ignite under clearly defined conditions and, moreover, are only mechanically resilient.
  • Another set of fog is known from DE-A-2 743 363. It contains zinc oxide, ammonium perchlorate, polychloroisoprene as well as a plasticizer and ammonium chloride for buffering. This mist set also has the disadvantage that carcinogenic combustion products are formed when it is burned off. Furthermore, the process for its production is very complex, since it is encapsulated and verse with two coatings for stabilization and protection against external influences must be hen.
  • the object of the invention is to provide a pyrotechnic charge as a smoke or as a fire in the form of a layered compact in a shell provided with longitudinal target breaking points with a central recess in which a primer is arranged, which is easy and inexpensive to manufacture and a better distribution which enables ignited fog or incendiary devices.
  • Another object of the invention is to provide a new mixture of a fog, fire and primer, and methods for their production, which is improved over the prior art.
  • the object is achieved by a pyrotechnic charge as a fog or as a fire in the form of layered stacked pressed bodies with a central recess in a shell with longitudinal target breaking points, in which an ignition charge is arranged, in that the shell also has transverse target breaking points that the pressing bodies are disc-shaped and the recess are cross-shaped and star-shaped, and that the primer is space-filling in the channel formed by the recesses.
  • Such a shell bursts easily after ignition and therefore ensures a better distribution of the fog or incendiary charges, in addition, only small parts of the shell remain, so that there is no risk of injury. Due to the space-filling arrangement of the ignition charges, an additional ignition tube is unnecessary and the friction between the individual pressing bodies is excluded.
  • Pyrotechnic charges as a fog set are preferred from claims 2 to 5, a method for their production from claim 6.
  • a preferred pyrotechnic charge is set as a fire and in claim 10, an advantageous method for its production.
  • Claims 9 to 14 represent preferably ignition charges to be used for the pyrotechnic charges according to the invention, claim 15 represents an advantageous method for their production.
  • a pyrotechnic charge as a smoke or incendiary charge is arranged in a preferably cylindrical shell 1.
  • the envelope 1 (FIG. 1) is provided with longitudinal and / or transverse breaking points 2. These can be produced as notches or fracture lines on the inside of the casing 1 or in the form of material dilutions.
  • the shell 1 is made of a plastic, but can also be made of a light metal such. B. aluminum or light metal alloys.
  • the mist or incendiary mixtures are stacked on top of one another as disk-shaped pressing bodies 3.
  • the outside diameter and the shape of the disk-shaped pressing bodies correspond to the inside diameter and the shape of the casing 1.
  • the pressing bodies 3 have recesses 4, which are preferably arranged axially symmetrically and enclose the central area. 1 and 2 cross-shaped recesses 4 are shown, but they can also be designed in a star shape with any number of points or rounded in a leaf shape.
  • the parts of the recesses 4 facing the outer edge simultaneously form predetermined breaking points 5 when the pressing bodies 3 are disassembled, so that the recesses 4 form a continuous channel 6 by means of a removable centering rod which reflects the shape of the recesses 4.
  • space-filling ignition molded bodies 7 are introduced into the channel 6. Due to the shape of the pressing body 4, the shell 1 is filled without gaps, a central internal ignition tube being superfluous.
  • the channel 6 formed is also completely filled by means of the ignition charge compression body 7, so that premature crumbling of the load during transport is excluded and there is direct contact between the ignition charge and the fog or fire charge.
  • the disk-shaped pressing bodies are easy to manufacture and just as easy to insert into the casing.
  • the ignition charge compression bodies 7 burn, ignite the compression bodies 3 of the fog or incendiary charge, which burst at the predetermined breaking points 5 given by the recesses 4, whereupon the casing 1 at the predetermined breaking points 2 arranged there due to the increasing internal pressure bursts.
  • the individual parts of the press body 3 of the mist or incendiary device are further broken down and distributed in all directions.
  • the three components of primer, mist or incendiary and casing therefore work together optimally in that the ignition and pressure build up occur at the same time.
  • the individual parts are distributed over a definable field. B. a homogeneous fog is generated.
  • the fog or the fire segments are quickly and permanently generated.
  • the fog or fire time can be controlled by varying the thickness of the pressed bodies and, in particular, by varying their composition, with different burn-off times being achieved.
  • mist set which has the following compositions in% by weight:
  • Preferred binders are an elastomer or a rubber-based polymer.
  • compositions in% by weight have the following compositions in% by weight:
  • the mist mixtures are produced in the form of compacts in that the components are mixed with one another with a solvent-containing binder, comminuted in a dry manner with a friction shredder and subsequently pressed to form compacts using a pressure of 500 to 1500 bar.
  • This process produces particularly stable compacts, which have a high mechanical strength and do not burst into small parts.
  • the high mechanical stability of the pressed body can be attributed to several factors. It results from the mixture of the individual components, from the completely irregular shape of the particles and their compression under pressure.
  • the bodies can be made in different sizes up to at least 155 caliber.
  • the firing time can be controlled by varying the thickness of the pressed body.
  • a batch of 2.2 kg of PVC powder, 3.3 kg of zinc oxide (dried), 2.2 kg of ammonium chloride and 2.64 kg of thiourea is pressed through a sieve with a mesh size of 0.3 to 0.55 mm and then intensely mixed. The mixture is then introduced into a kneading machine and pasted for 15 minutes with 2.4 kg (based on the solid portion, i.e. without solvent portion) of a highly viscous elastomer binder. After the kneading process is completed, ammonium perchlorate processed in the same sieving process is added in an amount of 7.26 kg.
  • This mixture is kneaded for a further 15 minutes, then spread out on trays and subsequently dried at a temperature of 45 ° C. for 6 hours.
  • the dry mass obtained is then comminuted in a grating machine and finally compressed to pressed bodies under a pressure of approximately 1000 bar.
  • a pyrotechnic charge as a fire charge has the following composition in% by weight:
  • the preparation takes place in such a way that the substances mentioned are introduced into a mixer without a binder and mixed with the binder, preferably an elastomer binder, and then granulated.
  • the finished granulate is dried on drying trays for 5 hours and then pressed into shaped articles.
  • the ignition kits for pyrotechnic charges which contain magnesium powder, black powder flour, an oxygen donor and a binder, have a magnesium powder with a grain size below 100 1 1m, preferably below, in order to obtain precise, defined and constant ignition conditions 60 1 1m and additional amorphous boron.
  • a catalyst preferably in the form of an iron (II) iron (III) complex, in particular iron blue, can additionally be provided to accelerate the burning off.
  • Solid chlorinated paraffin serves as a binder.
  • Ignition charges according to the invention have the following compositions in% by weight:
  • a preferred composition has in% by weight:
  • the components of the primer are mixed in a solvent, dried, granulated and then pressed into shaped articles using a pressure of 500 to 4000 bar.
  • the primers according to the invention are characterized by precise and constant ignition processes and a high mechanical strength.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Botany (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Air Bags (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Powder Metallurgy (AREA)
  • Disintegrating Or Milling (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

Described is a pyrotechnic charge as smoke- or combustion charge in the form of separate pressed objects arranged in a case, the improvement comprising the fact that the case (1) for the pressed objects (3) consists of plastic or light metal provided with preset breaking points (2). More specifically, the pyrotechnic charge contains a charge base containing smoke compounds in the form of pressed objects and also contains an igniting charge.

Description

Die Erfindung betrifft eine pyrotechnische Ladung als Nebel- oder Brandsatz in Form von in einer mit Längssollbruchstellen versehenen Hülle schichtförmig gestapelten Preßkörpern mit zentraler Aussparung, in der ein Anzündsatz angeordnet ist, sowie Verfahren zu deren Herstellung.The invention relates to a pyrotechnic charge in the form of smoke or incendiary charges in the form of pressed bodies stacked in layers in a shell provided with longitudinal target breaking points and having a central recess in which an ignition charge is arranged, and methods for their production.

Es sind zahlreiche Arten von nebelerzeugenden Stoffen oder Stoffgemischen sowie Vorrichtungen, welche sie in ein oder über ein Zielgebiet verschießen, bekannt. Üblicherweise werden die Nebelmischungen geformt und zu Preßkörpern verpreßt, in einer Metallhülse gestapelt und bei Zündung gegebenenfalls unter Verwendung eines Anzündsatzes aus der Hülsenöffnung ausgestoßen, wobei sie sich wie ein Schrotschuß kegelförmig verteilen.Numerous types of mist-producing substances or mixtures of substances and devices which fire them into or over a target area are known. Usually, the mist mixtures are shaped and pressed into compacts, stacked in a metal sleeve and, if ignited, ejected from the sleeve opening, if necessary using an igniter, whereby they are distributed conically like a shot.

Aus der DE-A-2412346 ist ein Brandsatz mit den Merkmalen des Oberbegriffs des Anspruchs 1 bekannt, der zum Abschuß aus einem Handabfeuerungsgerät vorgesehen ist. Hierbei ist die Hülle so ausgelegt, daß sie sich bei einem Aufprall im wesentlichen über die gesamte Länge mechanisch zerlegt. In der zentralen Aussparung ist ein Metallröhrchen angeordnet, in dem der ein Glühsatz und ein Zerlegersatz aneinander angrenzend angeordnet sind, wobei die Wandung des Metallröhrchens im Bereich des Glühsatzes verstärkt ist.From DE-A-2412346 a fire set with the features of the preamble of claim 1 is known, which is provided for firing from a hand-held device. Here, the shell is designed so that it collapses mechanically over its entire length in the event of an impact. A metal tube is arranged in the central recess, in which a glow plug and a disassembly set are arranged adjacent to one another, the wall of the metal tube being reinforced in the area of the glow plug.

Aus der DE-A-1 913 790 ist eine Vorrichtung zur Erzeugung einer künstlichen Nebeldecke bekannt, in welcher die Preßkörper in einer berstsicheren Hülle um ein Zündrohr gestapelt sind. Diese Vorrichtung weist erhebliche Nachteile auf. So wird der Raum in der Hülle durch die in ihr gestapelten segmentierten Preßkörper nicht optimal genutzt. Vielmehr liegen Hohlräume vor, welche die Ladungsdichte vermindern. Außerdem entsteht insbesondere bei der Herstellung und beim Transport durch Abrieb an den Grenzflächen der Preßkörper ein erhöhter Staubanteil im Nebelsatz, der die Wirkung herabsetzende Materialverlust bewirkt. Schließlich ist auch der fertigungstechnische Aufwand sowohl zur Herstellung der segmentierten Preßkörper, als auch zu deren Einfügung in eine Ladungshülle unter Verwendung eines Zündrohres erheblich.From DE-A-1 913 790 a device for producing an artificial fog blanket is known, in which the pressing bodies are stacked in a burst-proof envelope around an ignition tube. This device has considerable disadvantages. The space in the casing is therefore not optimally used due to the segmented pressing bodies stacked in it. Rather, there are cavities that reduce the charge density. In addition, an increased amount of dust in the mist set, which causes the effect of reducing material loss, arises in particular during manufacture and during transport due to abrasion at the interfaces of the pressed bodies. Finally, the manufacturing outlay is also considerable, both for producing the segmented pressing bodies and for inserting them into a charge envelope using an ignition tube.

Weitere Nachteile derartiger bekannter pyrotechnischer Ladungen resultieren aus dem Ausstoßprinzip. Da der Ausstoß der Preßkörper nur in einer Richtung erfolgt, ist zwangsläufig eine Begrenzung der Flächenbelegung vorgegeben. Die Flächenbelegung ist damit immer von der Ausstoßhöhe abhängig und kann bei schrotschußartiger Ausstoßung nicht variiert werden, was insbesondere bei Nebelsätzen nachteilig ist, aber auch bei Brandsätzen von Bedeutung sein kann.Further disadvantages of such known pyrotechnic charges result from the ejection principle. Since the pressing bodies are only ejected in one direction, a limitation of the area occupancy is inevitable. The area coverage is therefore always dependent on the discharge height and cannot be varied in the case of discharge shot-like, which is disadvantageous in particular in the case of mist sets, but can also be important in the case of incendiary sets.

Ferner entsteht durch den Ausstoß in einer Richtung aufgrund der Reibung der Preßkörper entlang der Hülle ein weiterer Materialverlust. Außerdem sind die Einzelsegmente derart beschaffen, daß sie durch die bei der Zündung auftretende Druckbelastung teilweise zu kleinen Partikeln zerstört werden.Furthermore, there is a further loss of material due to the ejection in one direction due to the friction of the pressing bodies along the casing. In addition, the individual segments are designed in such a way that they are partially destroyed into small particles by the pressure load that occurs during ignition.

Ein weiterer Nachteil der bekannten Ladungen liegt in der zentralen Anordnung eines zusätzliche Kosten erzeugenden Rohres als Zündrohr, wodurch ein unmittelbarer Kontakt zwischen Anzündsäule und Nebelkörpern nicht gegeben ist.Another disadvantage of the known charges lies in the central arrangement of an additional cost-generating tube as an ignition tube, as a result of which there is no direct contact between the igniter column and fog bodies.

Die meist aus Metall bestehende Hülle, aus welcher die Nebel- oder Brandsätze in einer bestimmten Höhe ausgestoßen werden, fällt anschließend unzerstört als ein Teil zu Boden und kann unter ungünstigen Umständen auch erhebliche Verletzungen hervorrufen.The shell, usually made of metal, from which the smoke or incendiary devices are ejected at a certain height, then falls undamaged as a part to the ground and can also cause serious injuries under unfavorable circumstances.

Ein weiterer Nachteil der bekannten, als Nebelsatz verwendeten Ladungen rührt von der Zusammensetzung der Nebelmischung her. Diese reagieren häufig sauer bzw. entwickeln Phosphorpentoxid, welches an der Luft zu Phosphorsäure umgesetzt wird, rufen Atembeschwerden und Hustenreiz hervor oder greifen innere Organe an. Derartige Nachteile sind besonders unerwünscht, wenn man an die Verwendung von Nebelladungen in Weinanbaugebieten zur Frostverhinderung oder bei Anwendung zu Übungs- und Manöverzwecken denkt.Another disadvantage of the known charges used as a mist set arises from the composition of the mist mixture. These often react acidic or develop phosphorus pentoxide, which is converted to phosphoric acid in the air, cause breathing difficulties and coughing or attack internal organs. Such disadvantages are particularly undesirable when one thinks of the use of fog loads in wine-growing areas to prevent frost or when used for training and maneuvering purposes.

Bekannt sind auch verschiedene Rauch- und Nebelmischungen. Beispielsweise wird in der DE-B-2451 701 ein Rauch- oder Nebelsatz beschrieben, der einen organischen Chlordonator, Metallpulver und/oder Metalloxid enthält. Der bekannte Nebelsatz enthält als Bindemittel mindestens einen der hochmolekularen Chlordonatoren Chlorparaffin, chloriertes Polyphenylen, chloriertes Polyphenoxyharz und Polyester aus Tetrachlorphthalsäure mit chloriertem Polyalkohol.Various smoke and fog mixtures are also known. For example, DE-B-2451 701 describes a smoke or mist set which contains an organic chlorine donor, metal powder and / or metal oxide. The known mist set contains at least one of the high molecular weight chlorine donors chloroparaffin, chlorinated polyphenylene, chlorinated polyphenoxy resin and polyester from tetrachlorophthalic acid with chlorinated polyalcohol as a binder.

Nachteilig bei diesen bekannten Nebelsätzen sind deren Hustenreiz verursachende und in Abhängigkeit von der genauen Zusammensetzung mehr oder weniger toxische Eigenschaften. Andere Rauch- und Nebelsätze bestehen aus einer Mischung von Hexachloräthan mit Metallpulver, wie Zink, Aluminium, Titan, Magnesium und Eisen.A disadvantage of these known mist sets are their coughing and, depending on the exact composition, more or less toxic properties. Other smoke and mist sets consist of a mixture of hexachloroethane with metal powder such as zinc, aluminum, titanium, magnesium and iron.

Diese Mischungen weisen den Nachteil auf, daß das Hexachloräthan sehr hydrolyseempfindlich ist und leicht bereits im Herstellungsprozeß mit Wasserdampf oder Feuchtigkeit reagiert. Darüber hinaus sind derartige Mischungen wenig lagerstabil und neigen zu Brennzeitänderungen.These mixtures have the disadvantage that the hexachloroethane is very sensitive to hydrolysis and easily reacts with water vapor or moisture already in the manufacturing process. In addition, such mixtures are not very stable in storage and tend to change the burning time.

Übliche Anzündsätze für Brand- oder Nebelsätze weisen als Hauptbestandeil Magnesiumpulver, Schwarzpulvermehl und ein Bindemittel auf. Sie besitzen den Nachteil, daß sie nicht unter eindeutig zu definierenden Bedingungen zünden und darüber hinaus nur gering mechanisch belastbar sind.Usual igniter sets for fire or smoke sets contain magnesium powder, black powder flour and a binding agent as main components. They have the disadvantage that they do not ignite under clearly defined conditions and, moreover, are only mechanically resilient.

Ein weiterer Nebelsatz ist aus der DE-A-2 743 363 bekannt. Als Bestandteile weist er Zinkoxid, Ammoniumperchlorat, Polychlorisopren sowie einen Weichmacher und zur Abpufferung Ammoniumchlorid auf. Auch dieser Nebelsatz weist den Nachteil auf, daß beim Abrennen cancerogene Verbrennungsprodukte entstehen. Ferner ist das Verfahren zu seiner Herstellung sehr aufwendig, da er vergossen und mit zwei Überzügen zur Stabilisierung und zum Schutz gegen äußere Einflüsse versehen werden muß.Another set of fog is known from DE-A-2 743 363. It contains zinc oxide, ammonium perchlorate, polychloroisoprene as well as a plasticizer and ammonium chloride for buffering. This mist set also has the disadvantage that carcinogenic combustion products are formed when it is burned off. Furthermore, the process for its production is very complex, since it is encapsulated and verse with two coatings for stabilization and protection against external influences must be hen.

Aufgabe der Erfindung ist es, eine pyrotechnische Ladung als Nebel- oder als Brandsatz in Form von in einer mit Längssollbruchstellen versehenen Hülle schichtförmig gestapelten Preßkörpern mit zentraler Aussparung, in der ein Anzündsatz angeordnet ist, anzugeben, die einfach und billig herstellbar ist und eine bessere Verteilung der gezündeten Nebel- oder Brandsätze ermöglicht.The object of the invention is to provide a pyrotechnic charge as a smoke or as a fire in the form of a layered compact in a shell provided with longitudinal target breaking points with a central recess in which a primer is arranged, which is easy and inexpensive to manufacture and a better distribution which enables ignited fog or incendiary devices.

Eine weitere Aufgabe der Erfindung ist es, eine gegenüber dem Stand der Technik verbesserte neue Mischung eines Nebel-, Brand- und Zündsatzes sowie Verfahren zu deren Herstellung bereitzustellen.Another object of the invention is to provide a new mixture of a fog, fire and primer, and methods for their production, which is improved over the prior art.

Die Aufgabe wird durch eine pyrotechnische Ladung als Nebel- oder als Brandsatz in Form von in einer Hülle mit Längssollbruchstellen versehenen schichtförmig gestapelten Preßkörpern mit zentraler Aussparung, in der ein Anzündsatz angeordnet ist, dadurch gelöst, daß die Hülle auch Quersollbruchstellen aufweist, daß die Preßkörper scheibenförmig und deren Aussparung kreuz- und sternförmig gestaltet sind, und daß der Anzündsatz raumfüllend in dem durch die Aussparungen gebildeten Kanal angeordnet ist.The object is achieved by a pyrotechnic charge as a fog or as a fire in the form of layered stacked pressed bodies with a central recess in a shell with longitudinal target breaking points, in which an ignition charge is arranged, in that the shell also has transverse target breaking points that the pressing bodies are disc-shaped and the recess are cross-shaped and star-shaped, and that the primer is space-filling in the channel formed by the recesses.

Eine derartige Hülle zerbirst leicht nach der Zündung und sichert daher eine bessere Raumverteilung der Nebel- bzw. Brandsätze, außerdem verbleiben nur kleine Hüllenteile, so daß eine Verletzungsgefahr dadurch nicht gegeben ist. Durch die raumfüllende Anordnung der Anzündsätze erübrigt sich ein zusätzliches Zündrohr und es wird die Reibung zwischen den einzelnen Preßkörpern ausgeschlossen.Such a shell bursts easily after ignition and therefore ensures a better distribution of the fog or incendiary charges, in addition, only small parts of the shell remain, so that there is no risk of injury. Due to the space-filling arrangement of the ignition charges, an additional ignition tube is unnecessary and the friction between the individual pressing bodies is excluded.

Bevorzugt pyrotechnische Ladungen als Nebelsatz sind den Ansprüchen 2 bis 5, ein Verfahren zu deren Herstellung dem Anspruch 6 zu entnehmen.Pyrotechnic charges as a fog set are preferred from claims 2 to 5, a method for their production from claim 6.

Im Anspruch 7 ist eine bevorzugte pyrotechnische Ladung als Brandsatz und in Anspruch 10 ein vorteilhaftes Verfahren zu deren Herstellung angegeben.In claim 7, a preferred pyrotechnic charge is set as a fire and in claim 10, an advantageous method for its production.

Die Ansprüche 9 bis 14 geben vorzugsweise für die erfindungsgemäßen pyrotechnischen Ladungen zu verwendende Anzündsätze wieder, Anspruch 15 gibt ein vorteilhaftes Verfahren zu deren Herstellung wieder.Claims 9 to 14 represent preferably ignition charges to be used for the pyrotechnic charges according to the invention, claim 15 represents an advantageous method for their production.

Nachstehend wird die Erfindung anhand von Ausführungsbeispielen unter Bezug auf Zeichnungen näher erläutert. Es zeigt

  • Fig. 1 eine pyrotechnische Ladung aus Preßkörpern mit Anzündsatz in einer Hülle,
  • Fig. 2a einen Preßkörper in perspektivischer Darstellung,
  • Fig. 2b-d die Zerlegung eines Preßkörpers nach dem Zünden des Zündsatzes in Draufsicht.
The invention is explained in more detail below using exemplary embodiments with reference to drawings. It shows
  • 1 is a pyrotechnic charge from pressed bodies with an ignition charge in a shell,
  • 2a shows a pressing body in a perspective view,
  • Fig. 2b-d the disassembly of a compact after igniting the primer in plan view.

Eine pyrotechnische Ladung als Nebel- oder Brandsatz ist in einer vorzugsweise zylindrischen Hülle 1 angeordnet. Die Hülle 1 (Fig. 1) ist mit Längs- und/oder Quersollbruchstellen 2 versehen. Diese können als an der Innenseite der Hülle 1 ausgeführte Kerben oder Bruchlinien oder in Form von Materialverdünnungen hergestellt sein. Die Hülle 1 besteht aus einem Kunststoff, kann aber auch aus einem Leichtmetall wie z. B. Aluminium oder aus Leichtmetall-Legierungen bestehen.A pyrotechnic charge as a smoke or incendiary charge is arranged in a preferably cylindrical shell 1. The envelope 1 (FIG. 1) is provided with longitudinal and / or transverse breaking points 2. These can be produced as notches or fracture lines on the inside of the casing 1 or in the form of material dilutions. The shell 1 is made of a plastic, but can also be made of a light metal such. B. aluminum or light metal alloys.

In der Hülle 1 sind die Nebel- oder Brandsatzmischungen als scheibenförmige Preßkörper 3 aufeinandergestapelt angeordnet. Der Außendurchmesser und die Gestalt der scheibenförmigen Preßkörper entspricht dem Innendurchmesser und der Gestalt der Hülle 1. Die Preßkörper 3 weisen Aussparungen 4 auf, die vorzugsweise achssymmetrisch angeordnet und den zentralen Bereich einschließen. In Fig. 1 und 2 sind kreuzförmige Aussparungen 4 dargestellt, sie können aber auch sternförmig mit beliebiger Zackenzahl oder auch blattförmig gerundet ausgeführt sein.In the casing 1, the mist or incendiary mixtures are stacked on top of one another as disk-shaped pressing bodies 3. The outside diameter and the shape of the disk-shaped pressing bodies correspond to the inside diameter and the shape of the casing 1. The pressing bodies 3 have recesses 4, which are preferably arranged axially symmetrically and enclose the central area. 1 and 2 cross-shaped recesses 4 are shown, but they can also be designed in a star shape with any number of points or rounded in a leaf shape.

Die zum Außenrand weisenden Teile der Aussparungen 4 bilden gleichzeitig Sollbruchstellen 5 beim Zerlegen der Preßkörper 3 werden derart mittels eines entfernbaren Zentrierstabes, der die Form der Aussparungen 4 wiedergibt, übereinander geschichtet, daß die Aussparungen 4 einen durchgehenden Kanal 6 bilden. In den Kanal 6 werden anschließend raumfüllende Anzündsatzpreßkörper 7 eingeführt. Durch die Gestalt der Preßkörper 4 wird die Hülle 1 lückenlos gefüllt, wobei ein zentrales Innenzündrohr überflüssig wird. Der gebildete Kanal 6 wird ebenfalls lückenlos mittels der Anzündsatzpreßkörper 7 gefüllt, so daß ein vorzeitiges Verkrümeln der Ladung beim Transport ausgeschlossen ist und ein unmittelbarer Kontakt zwischen Anzündsatz und Nebel- bzw. Brandsatz gegeben ist. Die scheibenförmigen Preßkörper sind leicht herzustellen und ebenso leicht in die Hülle einzubringen.The parts of the recesses 4 facing the outer edge simultaneously form predetermined breaking points 5 when the pressing bodies 3 are disassembled, so that the recesses 4 form a continuous channel 6 by means of a removable centering rod which reflects the shape of the recesses 4. Subsequently, space-filling ignition molded bodies 7 are introduced into the channel 6. Due to the shape of the pressing body 4, the shell 1 is filled without gaps, a central internal ignition tube being superfluous. The channel 6 formed is also completely filled by means of the ignition charge compression body 7, so that premature crumbling of the load during transport is excluded and there is direct contact between the ignition charge and the fog or fire charge. The disk-shaped pressing bodies are easy to manufacture and just as easy to insert into the casing.

Im Zeitpunkt der Zündung der Ladung brennen die Anzündsatzpreßkörper 7 durch, entzünden die Preßkörper 3 des Nebel- bzw. Brandsatzes, die an den durch die Aussparungen 4 vorgegebenen Sollbruchstellen 5 zerbersten, worauf aufgrund des stärker werdenden Innendruckes die Hülle 1 an den dort angeordneten Sollbruchstellen 2 zerbirst. Dadurch werden die Einzelteile der Preßkörper 3 des Nebel- bzw. Brandsatzes weiter zerlegt und in alle Richtungen verteilt. Die drei Komponenten Anzündsatz, Nebel- bzw. Brandsatz und Hülle wirken also auch insofern optimal zusammen, als Anzündung und Druckaufbau zum selben Zeitpunkt eintreten. Je nach vorgegebener und variabler Zerlegungsenergie verteilen sich die Einzelteile über ein definierbares Feld, wobei z. B. ein homogener Nebel erzeugt wird.At the time of ignition of the charge, the ignition charge compression bodies 7 burn, ignite the compression bodies 3 of the fog or incendiary charge, which burst at the predetermined breaking points 5 given by the recesses 4, whereupon the casing 1 at the predetermined breaking points 2 arranged there due to the increasing internal pressure bursts. As a result, the individual parts of the press body 3 of the mist or incendiary device are further broken down and distributed in all directions. The three components of primer, mist or incendiary and casing therefore work together optimally in that the ignition and pressure build up occur at the same time. Depending on the specified and variable decomposition energy, the individual parts are distributed over a definable field. B. a homogeneous fog is generated.

Der Nebel bzw. die Brandsegmente werden schnell und gleichzeitig dauerhaft erzeugt. Die Nebel- bzw. Brandzeit läßt sich durch unterschiedliche Dicke der Preßkörper als auch insbesondere durch Variation ihrer Zusammensetzung, wobei unterschiedliche Abbrandzeiten erreicht werden, steuern.The fog or the fire segments are quickly and permanently generated. The fog or fire time can be controlled by varying the thickness of the pressed bodies and, in particular, by varying their composition, with different burn-off times being achieved.

Die Nachteile bekannter Nebelmischungen, wie saure Reaktion der Nebelpartikel, Lagerinstabilität und Neigung zu Brennzeitänderungen, werden durch einen Nebelsatz vermieden, der folgende Zusammensetzungen in Gew.-% aufweist:

Figure imgb0001
The disadvantages of known mist mixtures, such as acid reaction of the mist particles, storage instability and tendency to change the burning time, are avoided by a mist set which has the following compositions in% by weight:
Figure imgb0001

Bevorzugte Bindemittel sind ein Elastomer oder ein Polymerisat auf Kautschukbasis.Preferred binders are an elastomer or a rubber-based polymer.

Bevorzugte Zusammensetzungen von Nebelsätzen weisen folgende Zusammensetzungen in Gew.-% auf:

Figure imgb0002
Preferred compositions of fog sentences have the following compositions in% by weight:
Figure imgb0002

Erfindungsgemäß werden die Nebelmischungen in Form von Preßkörpern dadurch hergestellt, daß die Komponenten mit einem lösungsmittelhaltigen Bindemittel miteinander vermischt, getrocknet mit einem Reibschnitzler zerkleinert und nachfolgend unter Anwendung eines Druckes von 500 bis 1500 bar zu Preßkörpern verpreßt werden. Durch dieses Verfahren werden besonders stabile Preßkörper erzeugt, die eine hohe mechanische Belastbarkeit aufweisen und nicht in kleine Teile zerplatzen. Die hohe mechanische Stabilität der Preßkörper ist auf mehrere Faktoren zurückzuführen. Sie ergibt sich aus dem Gemisch der einzelnen Komponenten, aus der völlig unregelmäßigen Schnitzelform der Teilchen und ihrem Verpressen unter Druck. Die Körper sind in verschiedenen Größen bis zu mindestens 155er Kaliber herzustellen. Durch die Variation der Stärke der Preßkörper kann die Brennzeit gesteuert werden.According to the invention, the mist mixtures are produced in the form of compacts in that the components are mixed with one another with a solvent-containing binder, comminuted in a dry manner with a friction shredder and subsequently pressed to form compacts using a pressure of 500 to 1500 bar. This process produces particularly stable compacts, which have a high mechanical strength and do not burst into small parts. The high mechanical stability of the pressed body can be attributed to several factors. It results from the mixture of the individual components, from the completely irregular shape of the particles and their compression under pressure. The bodies can be made in different sizes up to at least 155 caliber. The firing time can be controlled by varying the thickness of the pressed body.

Nachstehend wird ein konkretes Ausführungsbeispiel der Herstellung von Preßkörpern eines Nebelsatzes angeführt.Below is a specific embodiment of the manufacture of moldings of a fog set.

Ein Ansatz von 2,2 kg PVC-Pulver, 3,3 kg Zinkoxid (getrocknet), 2,2 kg Ammoniumchlorid und 2,64 kg Thioharnstoff wird durch ein Sieb mit einer Maschenweite von 0,3 bis 0,55 mm gedrückt und anschließend intensiv vermischt. Sodann wird der Ansatz in eine Knetmaschine eingebracht und mit 2,4 kg (bezogen auf den festen Anteil, d. h. ohne Lösungsmittelanteil) eines hochviskosen Elastomerbinders 15 Minuten angeteigt. Nach Beendigung des Knetvorgangs wird nach demselben Siebverfahren bearbeitetes Ammoniumperchlorat in einer Menge von 7,26 kg zugegeben. Dieser Ansatz wird weitere 15 Minuten geknetet, sodann auf Horden ausgebreitet und nachfolgend 6 Stunden bei einer Temperatur von 45° C getrocknet. Anschließend wird die erhaltene Trockenmasse in einer Reibschnitzelmaschine zerkleinert und schließlich unter einem Druck von etwa 1000 bar zu Preßkörpern verpreßt.A batch of 2.2 kg of PVC powder, 3.3 kg of zinc oxide (dried), 2.2 kg of ammonium chloride and 2.64 kg of thiourea is pressed through a sieve with a mesh size of 0.3 to 0.55 mm and then intensely mixed. The mixture is then introduced into a kneading machine and pasted for 15 minutes with 2.4 kg (based on the solid portion, i.e. without solvent portion) of a highly viscous elastomer binder. After the kneading process is completed, ammonium perchlorate processed in the same sieving process is added in an amount of 7.26 kg. This mixture is kneaded for a further 15 minutes, then spread out on trays and subsequently dried at a temperature of 45 ° C. for 6 hours. The dry mass obtained is then comminuted in a grating machine and finally compressed to pressed bodies under a pressure of approximately 1000 bar.

Eine pyrotechnische Ladung als Brandsatz weist folgende Zusammensetzung in Gew.-% auf:

Figure imgb0003
A pyrotechnic charge as a fire charge has the following composition in% by weight:
Figure imgb0003

Die Herstellung erfolgt so, daß die genannten Substanzen ohne Bindemittel in einen Mischer eingebracht und mit dem Bindemittel, vorzugsweise einem Elastomerbinder, versetzt und dann granuliert werden. Das fertige Granulat wird 5 Stunden auf Trockenhorden getrocknet und anschließend zu Formkörpern verpreßt.The preparation takes place in such a way that the substances mentioned are introduced into a mixer without a binder and mixed with the binder, preferably an elastomer binder, and then granulated. The finished granulate is dried on drying trays for 5 hours and then pressed into shaped articles.

Die Anzündsätze für pyrotechnische Ladungen, die Magnesiumpulver, Schwarzpulvermehl, einen Sauerstoffdonator und ein Bindemittel enthalten, weisen, um präzise, definierte und konstante Zündbedingungen zu erhalten, ein Magnesiumpulver mit einer Korngröße unter 100 11m, vorzugsweise unter 60 11m und zusätzlich amorphes Bor auf. Zur Beschleunigung des Abbrennens kann zusätzlich ein Katalysator, vorzugsweise in Form eines Eisen(II)-Eisen(III)-Komplexes ― insbesondere Eisenblau - vorgesehen sein. Als Bindemittel dient festes Chlorparaffin.The ignition kits for pyrotechnic charges, which contain magnesium powder, black powder flour, an oxygen donor and a binder, have a magnesium powder with a grain size below 100 1 1m, preferably below, in order to obtain precise, defined and constant ignition conditions 60 1 1m and additional amorphous boron. A catalyst, preferably in the form of an iron (II) iron (III) complex, in particular iron blue, can additionally be provided to accelerate the burning off. Solid chlorinated paraffin serves as a binder.

Erfindungsgemäße Anzündsätze weisen folgende Zusammensetzungen in Gew.-% auf:

Figure imgb0004
Ignition charges according to the invention have the following compositions in% by weight:
Figure imgb0004

Eine bevorzugte Zusammensetzung weist in Gew.-% auf:

Figure imgb0005
A preferred composition has in% by weight:
Figure imgb0005

Die Komponenten des Anzündsatzes werden in einem Lösungsmittel vermischt, getrocknet, granuliert und nachfolgend unter Anwendung eines Preßdruckes von 500 bis 4000 bar zu Formkörpern verpreßt.The components of the primer are mixed in a solvent, dried, granulated and then pressed into shaped articles using a pressure of 500 to 4000 bar.

Nachstehend wird ein konkretes Ausführungsbeispiel der Herstellung von Preßkörpern eines Anzündsatzes angeführt.A specific embodiment of the production of molded parts of an ignition charge is given below.

In einem Mischbehälter werden 1,2 kg Magnesiumpulver und 0,9 kg Eisenblau gut untereinander vermischt. Zu dieser Vormischung gibt man 0,8 kg Chlorparaffin (pulverförmig), welches in 2 Liter Perchloräthylen gelöst wurde. Die Lösung wird mit der Vormischung in einem Mischer 10 Minuten gut vermengt. Danach gibt man 2,39 kg Bor amorph zu und wiederholt den Mischvorgang 5 Minuten. Als letzte Komponente gibt man 4,71 kg Schwarzpulvermehl (auf 2 Komponenten-Basis, d. h. ohne Schwefelzusatz) in das Mischgefäß und läßt nochmals 10 Minuten mischen. Danach wird der lösungsmittelfeuchte Satz durch ein 1,5 mm Sieb gerüttelt und auf Trockenhorden ausgebreitet. Nach einer Trokkenzeit von 5 Stunden bei 45° C kann der Satz mit einem Preßdruck von 1500 bar zu Stangen verpreßt werden.1.2 kg of magnesium powder and 0.9 kg of iron blue are mixed well with one another in a mixing container. 0.8 kg of chlorinated paraffin (powdered), which was dissolved in 2 liters of perchlorethylene, is added to this premix. The solution is mixed well with the premix in a mixer for 10 minutes. Then 2.39 kg of amorphous boron are added and the mixing process is repeated for 5 minutes. The last component is 4.71 kg of black powder flour (based on 2 components, i.e. without the addition of sulfur) in the mixing vessel and allowed to mix for another 10 minutes. Then the solvent-moist set is shaken through a 1.5 mm sieve and spread out on drying trays. After a drying time of 5 hours at 45 ° C the set can be pressed into bars with a pressure of 1500 bar.

Die erfindungsgemäßen Zündsätze zeichnen sich durch präzise und konstante Zündvorgänge und eine hohe mechanische Belastbarkeit aus.The primers according to the invention are characterized by precise and constant ignition processes and a high mechanical strength.

Claims (15)

1. Pyrotechnic charge as smoke or incendiary composition in the form of a sheath (1) provided with longitudinal places of preferred frangibility (2), press-moulded members (3) stacked in stratified configuration and having a central recess (4) in which an ignition composition is disposed, characterised in that the sheath (1) is also provided with transverse places of preferred frangibility, that the press-moulded members (3) are of disc shape their recesses (4) are of cruciform or star shaped configuration and that the ignition composition (7) is disposed in space-filling manner in the duct (6), which is formed by the recesses (4).
2. Pyrotechnica charge according to claim 1, functioning as smoke composition, containing a chlorine donator, metal oxide and ammonium chloride, characterised in that it has the following composition (in % by weight):
Figure imgb0012
3. Pyrotechnic charge as smoke composition according to claim 2, characterised in that an elastomer or a polymer based on rubber is used as binder.
4. Pyrotechnic charge as smoke composition according to claim 2 or 3, characterised in that it has the following composition (in % by weight):
Figure imgb0013
5. Pyrotechnic charge as smoke composition according to claim 2 or 3, characterised in that it has the following composition (in % by weight):
Figure imgb0014
6. Method for producing a pyrotechnic charge as a smoke composition according to any of the claims 2 to 5, in the form of pressmouldings characterised in that the components are mixed with a binder containing a solvent, are dried, are comminuted by means of a grater and are subsequently formed into pressmouldings by using a pressure of between 500 and 1500 bar.
7. Pyrotechnic charge according to claim 1, as incendiary composition, characterised in that it has the following composition (in % by weight):
Figure imgb0015
8. Method for producing a pyrotechnik charge as incendiary composition according to claim 7, characterised in that the substances are blended in a mixer with an elastomer binder, are granulated and are dried as finished granulates for 5 hours on drying racks and are subsequently pressed into mouldings.
9. Pyrotechnic charge according to any of the claims 1 to 5 or 7 with an ignition composition, containing magnesium powder, black powder meal, an oxygen donator and a binder, characterised in that the magnesium powder has a particle size of less than 100jim, preferably less than 60 µm.
10. Pyrotechnic charge according to claim 9, characterised in that the ignition composition additionally contains amorphous boron.
11. Pyrotechnic charge according to claim 9 or 10, characterised in that the ignition composition additionally contains a catalyst, more particularly in the form of an iron(II)-iron(III) complex, more particularly vivanite.
12. Pyrotechnic charge according to any of the claims 9 to 11, characterised in that the ignition composition contains solid chlorinated paraffin as binder.
13. Pyrotechnic charge according to any of the claims 9 to 12, characterised in that the ignition composition has the following composition (in % by weight):
Figure imgb0016
14. Pyrotechnic charge according to claim 13, characterised in that the ignition composition has the following composition (in % by weight):
Figure imgb0017
15. Method for producing an ignition composition according to any of the claims 9 to 14 with a pyrotechnic charge according to any of the claims 1 to 5 or 7, characterised in that the ignition mixture is mixed a binder containing solvent, is dried, granulated and subsequently, by the use of a compression pressure of 500 to 4000 bar, is compressed in a mould into a compression moulding.
EP81106031A 1980-08-20 1981-07-31 Pyrotechnic fog or smoke producing charge having a casing, its composition and method for its manufacture Expired EP0046230B1 (en)

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DE3031369A DE3031369C2 (en) 1980-08-20 1980-08-20 Pyrotechnic charge consisting of a smoke composition and an ignition charge and a method for producing the mist mixture and the ignition charge
DE3031369 1980-08-20

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Also Published As

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DE3031369C2 (en) 1987-01-02
US4474715A (en) 1984-10-02
DE3173299D1 (en) 1986-02-06
DE3031369A1 (en) 1982-02-25
EP0046230A2 (en) 1982-02-24
ATE17167T1 (en) 1986-01-15
EP0046230A3 (en) 1982-05-26

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