EP0226978B1 - Lamp having a glass bulb with a high silicic-acid content - Google Patents

Lamp having a glass bulb with a high silicic-acid content Download PDF

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Publication number
EP0226978B1
EP0226978B1 EP86117330A EP86117330A EP0226978B1 EP 0226978 B1 EP0226978 B1 EP 0226978B1 EP 86117330 A EP86117330 A EP 86117330A EP 86117330 A EP86117330 A EP 86117330A EP 0226978 B1 EP0226978 B1 EP 0226978B1
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EP
European Patent Office
Prior art keywords
glass
solder
lamp
bulb
solder glass
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
EP86117330A
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German (de)
French (fr)
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EP0226978A2 (en
EP0226978A3 (en
Inventor
Werner Dr. Weiss
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Osram GmbH
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Patent Treuhand Gesellschaft fuer Elektrische Gluehlampen mbH
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Publication of EP0226978A3 publication Critical patent/EP0226978A3/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01K—ELECTRIC INCANDESCENT LAMPS
    • H01K1/00—Details
    • H01K1/38—Seals for leading-in conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
    • H01J5/32—Seals for leading-in conductors
    • H01J5/38—Pinched-stem or analogous seals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/36—Seals between parts of vessels; Seals for leading-in conductors; Leading-in conductors
    • H01J61/366—Seals for leading-in conductors
    • H01J61/368—Pinched seals or analogous seals

Definitions

  • the invention relates to a lamp with a bulb made of high-silica glass and power supply lines, which are melted into the bulb in a vacuum-tight manner by means of foils, the SiO2 content of the high-silica glass being at least 96% by weight, and between each foil and the Piston glass an intermediate layer of solder glass is present.
  • the tightness of the melt between the molybdenum foil and the quartz glass can be improved by an intermediate layer.
  • a thin metal layer for example made of chrome (US Pat. No. 3,420,944) or a solder glass, for example made of lead phosphorus oxide (GB Pat. No. 1,485,378) to protect against molybdenum. to apply.
  • FR-PS 961 730 is also known, the large differences in the coefficient of thermal expansion (AK) between molybdenum (AK 50 ⁇ 10 ⁇ 7 K ⁇ 1) and quartz glass (AK 7 ⁇ 10 ⁇ 7 K ⁇ 1) by one or more
  • AK coefficient of thermal expansion
  • the vapor deposition of thin metal layers is associated with high costs for material and implementation of the technical process, while the lead phosphorus oxide glass is unsuitable for high temperatures.
  • the intermediate glasses which are adjusted with regard to the coefficient of expansion, are also unsuitable for high temperatures; moreover, the application of several intermediate layers is very complex.
  • the invention has for its object to improve the tightness of the melt in a lamp with a bulb made of high-silica glass and power supplies that are melted into the bulb in a vacuum-tight manner by means of foils, and an intermediate layer of solder glass being present between each foil and the bulb glass .
  • solder glass has the following main components SiO2 60 - 70 wt .-% Al2O3 3-20% by weight K2O 12-18% by weight and, apart from minor impurities, is free of Na2O.
  • the advantages achieved are that the intermediate layer withstands the exposure to temperature and chemical influences, such as occur with halogen lamps of high power, and thus the service life of these lamps is extended.
  • the solder glass according to the invention not only prevents oxidation of the foils, but also improves the wetting ability and the wetting speed of the quartz glass / molybdenum system. As a result of the greatly improved adhesive power, the lack of adaptation of the thermal expansion coefficient is meaningless.
  • the application of the glass solder does not require any additional pretreatment of the film.
  • the solder glass contains the following main components SiO2 66% by weight Al2O3 18% by weight K2O 15% by weight
  • solder glass can be obtained inexpensively directly from potassium feldspar.
  • the solder glass is particularly advantageously applied to the film in an amount of 5-10 mg / cm 2. A smaller amount could not guarantee the complete wetting of a larger coherent surface on the film, a larger amount would endanger the tightness of the melt due to the increasing layer thickness.
  • FIG. 1 shows a halogen lamp 1 of high power that is pinched on one side.
  • the coil 3 is fastened to the two inner power supply lines 4 and 5.
  • the inner power supply lines 4 and 5 are connected to the outer power supply lines 8 and 9 via molybdenum foils 6 and 7, respectively.
  • the coil 3 is made of tungsten
  • the power supply lines 4, 5, 8, 9 are made of molybdenum.
  • a broad transverse strip in the middle of the foils 6, 7 is provided with an approximately 20 ⁇ m thick layer 10, 11 of a solder glass according to the invention.
  • the end regions of the foils 6, 7, in which the power supply wires 4, 5, 8, 9 end, remain spared from the coating.
  • the piston 2 can be surrounded by an outer piston.
  • FIG. 2 shows an exemplary embodiment of a metal halide discharge lamp 12 pinched on two sides.
  • two electrodes 14, 15 are fastened to inner power supply lines 16, 17, which are melted into the two ends of the bulb 13 by means of the foils 18, 19.
  • the conductive connection from the foils 18, 19 to the outside takes place via the two outer power supply lines 20, 21.
  • the sealing is also sealed here by a layer 22, 23 which is applied in the middle of the foils 18, 19 as a transverse strip guaranteed a solder glass according to the invention.
  • a suspension is first formed from the solder glass and an organic carrier material, which is already connected to the current supply wires 4, 5, 8, 9; 16, 17, 20, 21 equipped foils 6, 7; 18, 19 is applied in a neutral atmosphere (N2).
  • N2 a neutral atmosphere
  • the suspension medium, the flask 2; 13 and the frames are heated as usual to approx. 2000 ° C and then squeezed.
  • the solder glass must be molten on the surface of the film, but without flowing off the film. The viscosity of the solder glass must therefore not be too low or too high.
  • solder glasses which have the following composition (data in% by weight).
  • Solder glass 1 consists of 15% K2O, 18% Al2O3, the rest SiO2.
  • Solder glass 2 consists of 16.1% K2O, 3.5% Al2O3, 64.7% SiO2; it also contains compatible components, especially alkaline earth oxides.
  • Solder glass 2 has a somewhat lower melting point than solder glass 1.
  • the coefficient of expansion of both solder glasses is about 80 ⁇ 10 ⁇ 7 K ⁇ 1.
  • the improved adhesive effect between the molybdenum foil and quartz glass due to the solder glass can be demonstrated by measuring the wetting angle of a quartz glass drop on a molybdenum foil. Without the intermediate layer of solder glass according to the invention - regardless of the type of quartz glass and one possible doping - a wetting angle of approx. 100 ° measured. The application of the intermediate layer leads to a considerable improvement in the wetting properties; the wetting angle was reduced to about 45 ° by both solder glasses.

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  • Vessels And Coating Films For Discharge Lamps (AREA)
  • Glass Compositions (AREA)

Description

Die Erfindung geht aus von einer Lampe mit einem Kolben aus hochkieselsäurehaltigem Glas und Stromzuführungen, die mittels Folien vakuumdicht in den Kolben eingeschmolzen sind, wobei der SiO₂-Gehalt des hochkieselsäurehaltigen Glases bei mindestens 96 Gew.-% liegt, und wobei zwischen jeder Folie und dem Kolbenglas eine Zwischenschicht aus Lotglas vorhanden ist.The invention relates to a lamp with a bulb made of high-silica glass and power supply lines, which are melted into the bulb in a vacuum-tight manner by means of foils, the SiO₂ content of the high-silica glass being at least 96% by weight, and between each foil and the Piston glass an intermediate layer of solder glass is present.

Die Technik der vakuumdichten Einschmelzung von Stromzuführung in den Kolben mittels Folien wird vornehmlich bei Halogenglühlampen und Metallhalogenidentladungslampen angewendet. Üblicherweise werden dabei Kolben aus Quarzglas und Folien aus Molybdän verwendet.The technique of vacuum-tight melting of the power supply in the bulb by means of foils is mainly used for incandescent lamps and metal halide discharge lamps. Pistons made of quartz glass and foils made of molybdenum are usually used.

Die Dichtheit der Einschmelzung zwischen der Molybdänfolie und dem Quarzglas läßt sich durch eine Zwischenschicht verbessern. Insbesondere ist es bekannt, auf die Molybdänfolie zum Schutz gegen Oxidation entweder eine dünne Metallschicht, z.B. aus Chrom, aufzudampfen (US-PS 3 420 944) oder ein Lotglas, z.B. aus Blei-Phosphor-Oxid (GB-PS 1 485 378), aufzutragen. Aus der FR-PS 961 730 ist außerdem bekannt, die großen Unterschiede im thermischen Ausdehnungskoeffizienten (A.K. ) zwischen Molybdän (A.K. 50 · 10⁻⁷ K⁻¹) und Quarzglas (A.K. 7 · 10⁻⁷ K⁻¹) durch eine oder mehrere Zwischenschichten von Gläsern mit hohem Boroxidgehalt, deren Ausdehnungskoeffizienten zwischen diesen beiden Extremwerten liegen, zu mildern.The tightness of the melt between the molybdenum foil and the quartz glass can be improved by an intermediate layer. In particular, it is known to vapor-coat either a thin metal layer, for example made of chrome (US Pat. No. 3,420,944) or a solder glass, for example made of lead phosphorus oxide (GB Pat. No. 1,485,378) to protect against molybdenum. to apply. From FR-PS 961 730 is also known, the large differences in the coefficient of thermal expansion (AK) between molybdenum (AK 50 · 10⁻⁷ K⁻¹) and quartz glass (AK 7 · 10⁻⁷ K⁻¹) by one or more To mitigate intermediate layers of glasses with a high boron oxide content, whose expansion coefficients lie between these two extreme values.

Das Aufdampfen dünner Metallschichten ist jedoch mit hohen Kosten für Material und Realisierung des technischen Ablaufs verbunden, während das BleiPhosphor-Oxid-Glas für hohe Temperaturen ungeeignet ist. Ebenso sind auch die bezüglich des Ausdehnungskoeffizienten angepaßten Zwischengläser für hohe Temperaturen ungeeignet, darüber hinaus ist das Anbringen mehrerer Zwischenschichten sehr aufwendig.The vapor deposition of thin metal layers is associated with high costs for material and implementation of the technical process, while the lead phosphorus oxide glass is unsuitable for high temperatures. Likewise, the intermediate glasses, which are adjusted with regard to the coefficient of expansion, are also unsuitable for high temperatures; moreover, the application of several intermediate layers is very complex.

Der Erfindung liegt die Aufgabe zugrunde, bei einer Lampe mit einem Kolben aus hochkieselsäurehaltigem Glas und Stromzuführungen, die mittels Folien vakuumdicht in den Kolben eingeschmolzen werden, und wobei zwischen jeder Folie und dem Kolbenglas eine Zwischenschicht aus Lotglas vorhanden ist, die Dichtheit der Einschmelzung zu verbessern.The invention has for its object to improve the tightness of the melt in a lamp with a bulb made of high-silica glass and power supplies that are melted into the bulb in a vacuum-tight manner by means of foils, and an intermediate layer of solder glass being present between each foil and the bulb glass .

Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß das Lotglas folgende Hauptbestandteile aufweist
SiO₂ 60 - 70 Gew.-%
Al₂O₃ 3 - 20 Gew.-%
K₂O 12 - 18 Gew.-%
und, abgesehen von geringen Verunreinigungen, frei von Na₂O ist.This object is achieved in that the solder glass has the following main components
SiO₂ 60 - 70 wt .-%
Al₂O₃ 3-20% by weight
K₂O 12-18% by weight
and, apart from minor impurities, is free of Na₂O.

Die erzielten Vorteile bestehen darin, daß die Zwischenschicht der Belastung durch Temperatur und chemische Einflüsse, wie sie bei Halogenlampen hoher Leistung auftreten, standhält und somit die Lebensdauer dieser Lampen verlängert wird. Das erfindungsgemäße Lotglas verhindert dabei nicht nur die Oxidation der Folien, sondern verbessert auch das Benetzungsvermögen und die Benetzungsgeschwindigkeit des Systems Quarzglas/Molybdän. Infolge des dadurch stark verbesserten Haftvermögens ist die fehlende Anpassung des thermischen Ausdehnungskoeffizienten bedeutungslos. Das Auftragen des Glaslots erfordert dabei keinerlei zusätzliche Vorbehandlung der Folie.The advantages achieved are that the intermediate layer withstands the exposure to temperature and chemical influences, such as occur with halogen lamps of high power, and thus the service life of these lamps is extended. The solder glass according to the invention not only prevents oxidation of the foils, but also improves the wetting ability and the wetting speed of the quartz glass / molybdenum system. As a result of the greatly improved adhesive power, the lack of adaptation of the thermal expansion coefficient is meaningless. The application of the glass solder does not require any additional pretreatment of the film.

In einer bevorzugten Ausführung enthält das Lotglas folgende Hauptkomponenten
SiO₂ 66 Gew.-%
Al₂O₃ 18 Gew.-%
K₂O 15 Gew.-%In a preferred embodiment, the solder glass contains the following main components
SiO₂ 66% by weight
Al₂O₃ 18% by weight
K₂O 15% by weight

In dieser bevorzugten Ausführung läßt sich das Lotglas direkt aus Kalifeldspat kostengünstig gewinnen.In this preferred embodiment, the solder glass can be obtained inexpensively directly from potassium feldspar.

Besonders vorteilhaft wird das Lotglas in einer Menge von 5-10 mg/cm² auf die Folie aufgetragen. Eine geringere Menge könnte die vollständige Benetzung einer größeren zusammenhängenden Fläche auf der Folie nicht garantieren, eine größere Menge würde infolge der zunehmenden Schichtdicke die Dichtheit der Einschmelzung gefährden.The solder glass is particularly advantageously applied to the film in an amount of 5-10 mg / cm 2. A smaller amount could not guarantee the complete wetting of a larger coherent surface on the film, a larger amount would endanger the tightness of the melt due to the increasing layer thickness.

Die Erfindung soll im folgenden näher erläutert werden.

Figur 1
zeigt eine einseitig gequetschte Halogenglühlampe entsprechend der Erfindung.
Figur 2
zeigt eine zweiseitig gequetschte Metallhalogenidentladungslampe entsprechend der Erfindung.
The invention will be explained in more detail below.
Figure 1
shows a pinched halogen incandescent lamp according to the invention.
Figure 2
shows a double-sided pinched metal halide discharge lamp according to the invention.

In Figur 1 ist eine einseitig gequetschte Halogenglühlampe 1 hoher Leistung gezeigt. Im Kolben 2 aus Quarzglas ist die Wendel 3 an den zwei inneren Stromzuführungen 4 bzw. 5 befestigt. Die inneren Stromzuführungen 4 bzw. 5 sind über Molybdänfolien 6 bzw. 7 mit den äußeren Stromzuführungen 8 bzw. 9 verbunden. Die Wendel 3 ist aus Wolfram, die Stromzuführungen 4, 5, 8, 9 sind aus Molybdän hergestellt. Um im Bereich der Quetschung bei Betriebstemperaturen von mehr als 400 °C die Vakuumdichtheit zu gewährleisten, ist jeweils ein breiter Querstreifen in der Mitte der Folien 6, 7 mit einer ca. 20 µm dicken Schicht 10, 11 eines Lotglases gemäß der Erfindung versehen. Die Endbereiche der Folien 6, 7, in denen die Stromzuführungsdrähte 4, 5, 8, 9 enden, bleiben dabei von der Beschichtung ausgespart. Um die Sicherheit beim Betrieb zu erhöhen, kann der Kolben 2 von einem Außenkolben umgeben sein.FIG. 1 shows a halogen lamp 1 of high power that is pinched on one side. In the piston 2 made of quartz glass, the coil 3 is fastened to the two inner power supply lines 4 and 5. The inner power supply lines 4 and 5 are connected to the outer power supply lines 8 and 9 via molybdenum foils 6 and 7, respectively. The coil 3 is made of tungsten, the power supply lines 4, 5, 8, 9 are made of molybdenum. In order to ensure vacuum tightness in the area of the pinch at operating temperatures of more than 400 ° C., a broad transverse strip in the middle of the foils 6, 7 is provided with an approximately 20 μm thick layer 10, 11 of a solder glass according to the invention. The end regions of the foils 6, 7, in which the power supply wires 4, 5, 8, 9 end, remain spared from the coating. In order to increase safety during operation, the piston 2 can be surrounded by an outer piston.

Ein Ausführungsbeispiel einer zweiseitig gequetschten Metallhalogenidentladungslampe 12 zeigt Fig. 2. Im Quarzglaskolben 13 sind zwei Elektroden 14, 15 an inneren Stromzuführungen 16, 17 befestigt, die mittels der Folien 18, 19 in die beiden Enden des Kolbens 13 eingeschmolzen sind. Die leitende Verbindung von den Folien 18, 19 nach außen erfolgt über die zwei äußeren Stromzuführungen 20, 21. Entsprechend dem ersten Ausführungsbeispiel ist auch hier die Dichtheit der Einschmelzung durch eine in der Mitte der Folien 18, 19 jeweils als Querstreifen angebrachte Schicht 22, 23 eines erfindungsgemäßen Lotglases gewährleistet.FIG. 2 shows an exemplary embodiment of a metal halide discharge lamp 12 pinched on two sides. In the quartz glass bulb 13, two electrodes 14, 15 are fastened to inner power supply lines 16, 17, which are melted into the two ends of the bulb 13 by means of the foils 18, 19. The conductive connection from the foils 18, 19 to the outside takes place via the two outer power supply lines 20, 21. According to the first exemplary embodiment, the sealing is also sealed here by a layer 22, 23 which is applied in the middle of the foils 18, 19 as a transverse strip guaranteed a solder glass according to the invention.

Für die Herstellung der Schicht 10, 11; 22, 23 wird zunächst aus dem Lotglas und einem organischen Trägermaterial eine Suspension gebildet, die auf die bereits mit den Stromzuführungsdrähten 4, 5, 8, 9; 16, 17, 20, 21 bestückten Folien 6, 7; 18, 19 in neutraler Atmosphäre (N₂) aufgetragen wird. Während einer Trocknungszeit von ca. 1-2 Minuten verdampft das Suspensionsmittel, der Kolben 2; 13 und die Gestelle werden wie üblich auf ca. 2000 °C erhitzt und dann gequetscht. Während des Quetschvorgangs muß dabei das Lotglas schmelzflüssig auf der Folienoberfläche vorliegen, ohne jedoch von der Folie abzufließen. Die Viskosität des Lotglases darf daher weder zu niedrig, noch zu hoch sein.For the production of the layer 10, 11; 22, 23, a suspension is first formed from the solder glass and an organic carrier material, which is already connected to the current supply wires 4, 5, 8, 9; 16, 17, 20, 21 equipped foils 6, 7; 18, 19 is applied in a neutral atmosphere (N₂). During a drying time of about 1-2 minutes, the suspension medium, the flask 2; 13 and the frames are heated as usual to approx. 2000 ° C and then squeezed. During the squeezing process, the solder glass must be molten on the surface of the film, but without flowing off the film. The viscosity of the solder glass must therefore not be too low or too high.

Diese Bedingung wird insbesondere von zwei Lotgläsern erfüllt, die folgende Zusammensetzung (Angaben in Gew.-%) aufweisen.
Lotglas 1 besteht aus 15 % K₂O, 18 % Al₂O₃, Rest SiO₂.
Lotglas 2 besteht aus 16,1 % K₂O, 3,5 % Al₂O₃,
64,7 % SiO₂; darüber hinaus enthält es kompatible Komponenten, insbesondere Erdalkalioxide.This condition is met in particular by two solder glasses which have the following composition (data in% by weight).
Solder glass 1 consists of 15% K₂O, 18% Al₂O₃, the rest SiO₂.
Solder glass 2 consists of 16.1% K₂O, 3.5% Al₂O₃,
64.7% SiO₂; it also contains compatible components, especially alkaline earth oxides.

Lotglas 2 besitzt im Vergleich zu Lotglas 1 einen etwas niedrigeren Schmelzpunkt. Der Ausdehnungskoeffizient beider Lotgläser beträgt etwa 80 · 10⁻⁷ K⁻¹.Solder glass 2 has a somewhat lower melting point than solder glass 1. The coefficient of expansion of both solder glasses is about 80 · 10⁻⁷ K⁻¹.

Die durch das Lotglas verbesserte Haftwirkung zwischen Molybdänfolie und Quarzglas läßt sich durch Messung des Benetzungswinkels eines Quarzglastropfens auf einer Molybdänfolie demonstrieren. Ohne die erfindungsgemäße Zwischenschicht aus Lotglas wurde - unabhängig von der Quarzglassorte und einer etwaigen Dotierung - ein Benetzungswinkel von ca. 100° gemessen. Das Auftragen der Zwischenschicht führt zu einer erheblichen Verbesserung der Benetzungseigenschaften; der Benetzungswinkel wurde durch beide Lotgläser auf etwa 45° reduziert.The improved adhesive effect between the molybdenum foil and quartz glass due to the solder glass can be demonstrated by measuring the wetting angle of a quartz glass drop on a molybdenum foil. Without the intermediate layer of solder glass according to the invention - regardless of the type of quartz glass and one possible doping - a wetting angle of approx. 100 ° measured. The application of the intermediate layer leads to a considerable improvement in the wetting properties; the wetting angle was reduced to about 45 ° by both solder glasses.

Claims (3)

  1. Lamp (1; 12) having a bulb (2; 13) of glass of a high silica content and having current supply leads (4, 5, 8, 9; 16, 17, 20, 21) which are fused vacuum-tightly into the bulb (2; 13) by means of foils (6, 7; 18, 19), the SiO₂ content of the glass of high silica content being at least 96% by weight and an intermediate layer (10, 11; 22, 23) of solder glass being present between each foil (6, 7; 18, 19) and the bulb glass, characterised in that the solder glass has the following main components, expressed in weight per cent:



            SiO₂ 60-70 %, Al₂O₃ 3-20 %, K₂O 12-18 %



    and, except for trace contaminants, is free from Na₂O.
  2. Lamp according to Claim 1, characterised in that the solder glass contains the following main components:



            SiO₂ 66 %, Al₂O₃ 18 %, K₂O 15 %.

  3. Lamp according to one of the preceding claims, characterised in that the solder glass is applied to the foil (6, 7; 18, 19) in a quantity of 5-10 mg/cm².
EP86117330A 1985-12-18 1986-12-12 Lamp having a glass bulb with a high silicic-acid content Expired - Lifetime EP0226978B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3544825 1985-12-18
DE19853544825 DE3544825A1 (en) 1985-12-18 1985-12-18 LAMP WITH A PISTON MADE OF GLASS, HIGH SILICA

Publications (3)

Publication Number Publication Date
EP0226978A2 EP0226978A2 (en) 1987-07-01
EP0226978A3 EP0226978A3 (en) 1989-06-14
EP0226978B1 true EP0226978B1 (en) 1991-12-27

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EP86117330A Expired - Lifetime EP0226978B1 (en) 1985-12-18 1986-12-12 Lamp having a glass bulb with a high silicic-acid content

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US (1) US4749902A (en)
EP (1) EP0226978B1 (en)
JP (1) JPS62147650A (en)
DE (2) DE3544825A1 (en)

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GB1485378A (en) * 1974-12-10 1977-09-08 Thorn Lighting Ltd Pinch foil seals
US4238705A (en) * 1979-09-12 1980-12-09 General Electric Company Incandescent lamp seal means
JPS5647142A (en) * 1979-09-25 1981-04-28 Toshiba Corp Detection system for error of transmitted data

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9567463B2 (en) 2011-09-30 2017-02-14 Basf Se High-strength blends based on polyarylene ethers

Also Published As

Publication number Publication date
EP0226978A2 (en) 1987-07-01
DE3544825A1 (en) 1987-06-19
JPS62147650A (en) 1987-07-01
US4749902A (en) 1988-06-07
EP0226978A3 (en) 1989-06-14
DE3683141D1 (en) 1992-02-06

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