EP0098858B1 - Power supply conductor, essentially for vacuum apparatus, and manufacturing method thereof - Google Patents

Power supply conductor, essentially for vacuum apparatus, and manufacturing method thereof Download PDF

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Publication number
EP0098858B1
EP0098858B1 EP83900433A EP83900433A EP0098858B1 EP 0098858 B1 EP0098858 B1 EP 0098858B1 EP 83900433 A EP83900433 A EP 83900433A EP 83900433 A EP83900433 A EP 83900433A EP 0098858 B1 EP0098858 B1 EP 0098858B1
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EP
European Patent Office
Prior art keywords
power supply
supply conductor
rhenium
molybdenum
line
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Expired
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EP83900433A
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German (de)
French (fr)
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EP0098858A4 (en
EP0098858A1 (en
Inventor
János NAGY
László NAGY
Endre Oldal
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Tungsram Rt
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Tungsram Rt
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Classifications

    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/32—Sealing leading-in conductors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12528—Semiconductor component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12597—Noncrystalline silica or noncrystalline plural-oxide component [e.g., glass, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12812—Diverse refractory group metal-base components: alternative to or next to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12826—Group VIB metal-base component

Definitions

  • the invention relates to a power entry line according to the preamble of claim 1 and a method for its production according to the preamble of claim 4.
  • the power entry line penetrating through the glass-like material is generally connected to a component made of any metal and this connection should have good electrical and mechanical properties.
  • a welding connection and in particular resistance welding is used most frequently for electrical light sources. Good weldability is therefore required.
  • Another requirement is that the Stromein enclosuresieitung with the glass-like material forms a hermetic seal.
  • Power supply lines made of molybdenum are often used in vacuum technology devices. The electrical current is fed, for example, to the burners of the high-pressure discharge lamps or the bulbs of the halogen incandescent lamps made of quartz glass through thin foils made of molybdenum.
  • molybdenum wires are also frequently used in the case of light sources with pistons made of tempered glass or of electron tubes.
  • hard-to-weld molybdenum is provided with a transition metal in a known manner or during welding, a separate coating metal element, for. B. a plate or a wire, the material of the coating metal is chosen such that the connection produced is of appropriate strength and toughness and these properties can be maintained even at higher operating temperatures of the devices.
  • a separate coating metal element for. B. a plate or a wire
  • the material of the coating metal is chosen such that the connection produced is of appropriate strength and toughness and these properties can be maintained even at higher operating temperatures of the devices.
  • these requirements such as, for example, with incandescent halogen lamps or metal halogen lamps
  • DE-A-3 104 043 also describes a method according to which the coating of the molybdenum foils is produced in the form of a metal layer by vacuum evaporation or atomization.
  • This application mentions platinum, tantalum, gold and rhenium as metals in which the process can in principle be used.
  • the thickness of the layer can take values from 20 to 10,000 nm.
  • the glass material can be hermetically sealed. Considering that the coating metal can only be profitable in a continuous process, this coating will be present in a continuous layer along the length of the power lead. The coating is therefore only reliable for carrying out a hermetically sealed connection if the glass-like material, in the molten or plastic state, is capable of wetting the coating material.
  • the noble metals such as B. platinum and gold, do not meet this requirement, and according to the experience of the applicant, it often happens with current conductors that are coated with a noble metal that the connection is not vacuum-tight or the device is vacuum-tight during storage or operation loses.
  • the object of the invention is to propose a metal coating which simultaneously ensures a particularly good weldability and ensures a hermetic seal with the glass-like material, moreover the treatment in hydrogen (in the editorial medium) is well tolerated and can be applied by a process which is as simple and quick as possible .
  • the invention is directed to a current introduction line, in particular for vacuum-technical apparatus, for example electrical light sources, the current introduction line serving to conduct the electrical current through a glass-like material and forming a hermetic seal with the glass-like material and furthermore the current introduction line consisting of molybdenum and at least on which the glass-like material comes into contact with the surface is provided with a metallic coating, which according to the invention consists of a rhenium layer.
  • the thickness of the rhenium layer is not a critical factor with regard to the solution of the task and that a rhenium layer of extremely small thickness (order of magnitude nm,) surprisingly considerably facilitates the weldability.
  • Electrolytic deposition is definitely inexpensive, i. H. compared with z. B. vacuum evaporation is a working method of low investment and relatively little loss of material.
  • the thickness of the rhenium layer is not a critical factor (although this can be controlled well by electrodeposition).
  • the molybdenum base metal has a foil shape and only the side to be welded has to be coated with rhenium
  • the side of the surface of the molybdenum base metal immersed in the electrolyte which lies opposite the area to be welded and should not be coated with rhenium is made out of one Support made or insulated with insulating material, expediently guided on a roller surface.
  • the covering of the molybdenum foil used for the quartz incandescent bodies of mercury lamps as the carrier metal of the power lead is described with a rhenium layer.
  • the film is 8.5 mm wide and 25 J lm thick and its edges - in a manner known per se - were thinned like knife edges by electrolytic etching.
  • This film then passes through a metal roller and then the lower lateral surface of a rotary roller with a diameter of 100 mm, which is made of insulating material or covered with insulating material, such as rubber.
  • the roller dips about 35 mm deep in the electrolyte and contains 10 g of KRe0 4 and 4 g of concentrated H 2 S0 4 dissolved in 1 liter of water.
  • the counter electrode is made of platinum and is connected to the positive terminal of the power source.
  • the negative terminal of the power source is connected to the metal roller that passed the film before immersing it in the electrolyte.
  • the speed of the forward transport of the film is selected so that the duration of the relevant point of the film in the electrolyte is about 30 seconds.
  • the electrolytic deposition should be carried out at room temperature, with a current density of about 800 A / m 2 .
  • the film emerging from the electrolysis bath passes through a washing system Water countercurrent, then a dryer with an air flow and a continuous furnace flushed with hydrogen at a temperature of 1100 ° C.
  • rhenium By means of the described arrangement it is achieved that only one side of the film is coated with rhenium. However, this is completely sufficient since, in the present application, the welding takes place only on one side of the film. Should the two sides or the wire be covered, this could easily be solved with the methods known per se.
  • the conditions for electrolytic deposition can be changed
  • baths with a composition that differs from the known can also be used.
  • the advantages of the current introduction line according to the invention consist in the fact that it can be welded particularly well, at the same time ensures the hermetic connection with the glass material, the heat treatment in the deoxidation medium, such as, for. B. well endured in hydrogen and besides these advantages can still be produced by a relatively inexpensive and simple process.

Abstract

Power supply conductor, essentially for vacuum apparatus, such as light electric sources, and which is used for transmitting electric power through a vitrous material, while providing for a sealed connection with said vitrous material. The base metal of the power supply conductor is molybdenum, coated with an intermediate metal layer on the whole surface or on the portion of the surface intended to be welded. The intermediate metal layer of the power supply conductor is comprised of rhenium with an appropriate thickness ranging from 3 to 1000 nm, preferably 10 to 100 nm. As an appropriate manufacturing method for the power supply conductor, there is proposed the electrolytic precipitation. The advantages of the power supply conductor which is proposed are the following: it lends itself to welding and provides at the same time for a sealed connection with the vitrous material, it withstands the thermal treatment in a reduction agent, such as hydrogen, and may be manufactured according to a relatively simple and inexpensive method.

Description

Die Erfindung betrifft eine Stromeinführungsleitung gemäß dem Oberbegriff des Patentanspruches 1 sowie ein Verfahren zu deren Herstellung gemäß dem Obergriff des Patentanspruches 4.The invention relates to a power entry line according to the preamble of claim 1 and a method for its production according to the preamble of claim 4.

Die an Stromeinführungsleitungen zu stellenden grundsätzlichen Anforderungen können wie folgt zusammengefasst werden:The basic requirements to be placed on power entry cables can be summarized as follows:

Die durch den glasartigen Werkstoff durchgreifende Stromeinführungsleitung ist im allgemeinen an einem aus irgendeinem Metall hergestellten Bestandteil angeschlossen und diese Verbindung soll über gute elektrische und mechanische Eigenschaften verfügen. Am häufigsten findet zum Beispiel bei elektrisch Lichtquellen eine Schweißverbindung und insbesondere eine Widerstandschweißung Anwendung. Es ist daher eine gute Schweißbarkeit erforderlich. Eine andere Anforderung besteht darin, daß die Stromeinführungsieitung mit dem glasartigen Werkstoff einen hermetischen Abschluß bildet. Bei vakuumtechnischen Geräten werden häufig Stromeinführungsleitungen aus Molybdän verwendet. Der elektrische Strom wird zum Beispiel den Brennkörpern der Hochdruckentladungslampen oder den aus Quarzglas gefertigten Kolben der Halogenglühlampen durch dünne Folien aus Molybdän zugeführt. Gleichfalls werden häufig Molybdändrähte auch im Falle von Lichtquellen mit Kolben aus Hartglas oder von Elektronröhren verwendet. Im Interesse der leichteren Schweißbarkeit und der besseren Qualität in bekannter Weise schwer schweißbare Molybdän mit einem Übergangsmetall versehen oder beim Schweißen wird zwischen die zu verschweißenden Flächen ein separates Überzugsmetallelement, z. B. eine Platte oder ein Draht gelegt, wobei das Material des Überzugsmetalls derart gewählt wird, daß die hergestellte Verbindung von entsprechender Festigkeit und Zähigkeit ist und diese Eigenschaften auch bei höheren Betriebstemperaturen der Geräte beibehalten werden können. Zu diesen Anforderungen kommt gegebenenfalls (wie z. B. bei Halogenglühlampen oder Metallhalogenlampen) noch die Anforderung der Beständigkeit gegen die Einwirkungen der Umgebungsatmosphären hinzu. In der Praxis ist als Überzugsmetall das Platin und das Tantal am meisten verbreitet, in der Literatur wird jedoch auch die Anwendung von Zirkonium, Niobium, Rhodium, Nickel, Gold, Palladium, sowie verschiedenen Legierungen erwähnt (s. z. B. W. Espe: "Materials of High Vacuum Technology", vol. 1., Ch. 9: Pergamon, 1966).The power entry line penetrating through the glass-like material is generally connected to a component made of any metal and this connection should have good electrical and mechanical properties. For example, a welding connection and in particular resistance welding is used most frequently for electrical light sources. Good weldability is therefore required. Another requirement is that the Stromeinführungsieitung with the glass-like material forms a hermetic seal. Power supply lines made of molybdenum are often used in vacuum technology devices. The electrical current is fed, for example, to the burners of the high-pressure discharge lamps or the bulbs of the halogen incandescent lamps made of quartz glass through thin foils made of molybdenum. Likewise, molybdenum wires are also frequently used in the case of light sources with pistons made of tempered glass or of electron tubes. In the interest of easier weldability and better quality, hard-to-weld molybdenum is provided with a transition metal in a known manner or during welding, a separate coating metal element, for. B. a plate or a wire, the material of the coating metal is chosen such that the connection produced is of appropriate strength and toughness and these properties can be maintained even at higher operating temperatures of the devices. In addition to these requirements (such as, for example, with incandescent halogen lamps or metal halogen lamps), there is also the requirement for resistance to the effects of the ambient atmospheres. In practice, platinum and tantalum are the most common coating metals, but the use of zirconium, niobium, rhodium, nickel, gold, palladium and various alloys is also mentioned in the literature (see BW Espe: "Materials of High Vacuum Technology ", vol. 1, Ch. 9: Pergamon, 1966).

Die Anwendung eines separaten Überzugsmetalls hat selbstverständlich zur Folge, daß beim Schweißvorgangs noch ein zusätzliches Element zugeführt und postioniert werden muß, wodurch das Verfahren verständlicher Weise komplizierter wird. Eine naheliegende Vereinfachung besteht darin, das Molybdän als Trägermetall - mindestens an der zu schweißenden Fläche - im voraus mit einem Metallüberzug zu versehen. So kann z. B. nach der FR-A-2 079 541 das vorherige Überziehen von Molybdänfolien derart ausgeführt werden, daß auf die Folie ein aus Platinenlegierung bestehender Überzug aufgetragen und dieser durch Wärmebehandlung zersetzt wird.Of course, the use of a separate coating metal means that an additional element has to be added and positioned during the welding process, which obviously makes the process more complicated. An obvious simplification is to provide the molybdenum as a carrier metal - at least on the surface to be welded - with a metal coating in advance. So z. B. according to FR-A-2 079 541, the previous coating of molybdenum foils is carried out in such a way that an existing coating of platinum alloy is applied to the foil and this is decomposed by heat treatment.

Aus der US-A-4 011 480 ist ferner eine Stromeinführungsleitung bekannt, die insgesamt aus Rhenium besteht und durch eine A1203-Keramikabdichtung hindurchgeführt ist.From US-A-4 011 480 a current lead is also known which consists entirely of rhenium and is passed through an A1 2 0 3 ceramic seal.

Die DE-A-3 104 043 beschreibt ferner ein Verfahren, wonach der Überzug der MolybdänFolien in Form einer Metallschicht durch Vakuumverdampfung oder Zerstäubung hergestellt wird. Diese Anmeldung erwähnt das Platin, das Tantal, das Gold und das Rhenium als Metalle, bei denen das Verfahren im Prinzip seine Anwendung finden kann. Die Dicke der Schicht kann Werte von 20 bis 10 000 nm annehmen.DE-A-3 104 043 also describes a method according to which the coating of the molybdenum foils is produced in the form of a metal layer by vacuum evaporation or atomization. This application mentions platinum, tantalum, gold and rhenium as metals in which the process can in principle be used. The thickness of the layer can take values from 20 to 10,000 nm.

Die wichtigste Anforderung an das Überzugsmetall besteht neben der leichten Schweißbarkeit darin, daß mit dem Glasmaterial ein hermetischer Abschluss ausgeführt werden kann. Mit Rücksicht darauf, daß das Auftragen des Überzugsmetalls nur bei einem kontinuierlichen Verfahren rentabel sein kann, wird dieser Überzug entlang der Länge der Stromeinführungsleitung in einer durchlaufenden Schicht vorhanden sein. Zur Ausführung einer hermetischen dichten Verbindung wird der Überzug daher nur dann zuverlässig, wenn der glasartige Stoff im geschmolzenen, beziehungsweise plastischen Zustand fähig ist, das Überzugsmaterial zu netzen. Die edlen Metalle, wie z. B. Platin und Gold, erfüllen diese Anforderung nicht, und nach den Erfahrungen der Anmelderin kommt es bei Stromleitern, die mit einem Edelmetall überzogen sind, häufig vor, daß die Verbindung nicht vakuumdicht ist oder das Gerät im Laufe der Lagerung oder des Betriebs seine Vakuumdichtheit verliert. Die Anforderung der Benetzung wird zwar durch Tantal befriedigt, bei der Anwendung von Tantal tritt jedoch die Schwierigkeit auf, daß das mit dem Überzug versehene Trägermetall im wasserstoffhaltigen Schutzgas nicht mehr behandelt werden kann, beziehungsweise falls dies trotzdem getan wird, wird die Stromeinführungsleitung für weitere Anwendung völlig ungeeignet. Diese Wärmebehandlung kann sich jedoch auch für zwei Zwecke als wünschenswert erweisen: einerseits zur Festigung der Verbindung zwischen der Überzugsmetallschicht und dem Trägermetall aus Molybdän durch Diffusion der beiden Materialien und andererseits zur Umwandlung der Fläche der Stromeinführungsleitung in einen definierten Zustand vor dem unmittelbaren Zustandebringen der Bindung zwischen Glas und Metall. Aus der Praxis ist nähmlich bekannt, daß, wenn z. B. die bei daß Quarglas-Abflaschungen gebräuchlichen Molybdänfolien nicht im frisch glühenden Zustand verwendet werden, sonder diese einige Tage in der Luft stehen, sich die Zuverlässigkeit der Bindung beträchtlich verringert. Im Falle einer unter ungeeigneten Umständen ausgeführten Schweißverbindung kann es vorkommen, daß die Oberfläche oxydiert, und bei solchen Fällen kann es notwendig sein, auch die aus der Stromeinführungsleitung und den daran angeschweissten Gegenständen bestehenden Armatur im wasserstoffhaltigen Medium (Reduktionsmedium) nachträglich zu erhitzen.In addition to being easy to weld, the most important requirement for the coating metal is that the glass material can be hermetically sealed. Considering that the coating metal can only be profitable in a continuous process, this coating will be present in a continuous layer along the length of the power lead. The coating is therefore only reliable for carrying out a hermetically sealed connection if the glass-like material, in the molten or plastic state, is capable of wetting the coating material. The noble metals, such as B. platinum and gold, do not meet this requirement, and according to the experience of the applicant, it often happens with current conductors that are coated with a noble metal that the connection is not vacuum-tight or the device is vacuum-tight during storage or operation loses. The wetting requirement is satisfied by tantalum, but when using tantalum there arises the difficulty that the carrier metal provided with the coating can no longer be treated in the hydrogen-containing protective gas, or if this is nevertheless done, the current introduction line becomes available for further use completely unsuitable. However, this heat treatment can also prove to be desirable for two purposes: on the one hand for strengthening the connection between the coating metal layer and the support metal made of molybdenum by diffusion of the two materials, and on the other hand for converting the area of the power lead into a defined state prior to the immediate formation of the bond between Glass and metal. From practice it is known that when z. B. the usual in that quar glass bottles Molybdenum foils are not used in the freshly glowing state, but they remain in the air for a few days, the reliability of the binding is considerably reduced. In the case of a welded joint which is carried out under unsuitable circumstances, it may happen that the surface is oxidized, and in such cases it may be necessary to subsequently heat the fitting consisting of the power inlet line and the objects welded to it in the hydrogen-containing medium (reducing medium).

Die Aufgabe der Erfindung besteht darin, einen Metallüberzug vorzuschlagen der gleichzeitige eine besondere gute Schweißbarkeit sichert und mit dem glasartigen Werkstoff einen hermetischen Abschluß gewährleistet, darüber hinaus die Behandlung im Wasserstoff (im Redaktionsmedium) gut erträgt und durch ein möglichst einfaches und schnelles Verfahren aufgetragen werden kann.The object of the invention is to propose a metal coating which simultaneously ensures a particularly good weldability and ensures a hermetic seal with the glass-like material, moreover the treatment in hydrogen (in the editorial medium) is well tolerated and can be applied by a process which is as simple and quick as possible .

Diese Aufgabe wird durch die kennzeichnenden Merkmale des Patentanspruches 1 bzw. 4 gelöst. Vorteilhafte Ausgestaltungen der Erfindung sind in den Unteransprüchen gekennzeichnet.This object is solved by the characterizing features of claim 1 or 4. Advantageous embodiments of the invention are characterized in the subclaims.

Der Erfindung ist dementsprechend auf eine Stromeinführungsleitung, insbesondere für vakuumtechnische Apparate, beispielweise elektrische Lichtquellen gerichtet, wobei die Stromeinführungsleitung die der Durchführung des elektrischen Stromes durch einen glasartigen Werkstoff dient und mit dem glasartigen Werkstoff einen hermetischen Abschluss bildet und ferner die Stromeinführungsleitung aus Molybdän besteht und zumindest an der mit dem glasartigen Werkstoff in Behrührung kommen den Oberfläche mit einem metallischen Überzug versehen ist, der erfindumgsgemäß aus einer Rheniumschicht besteht.Accordingly, the invention is directed to a current introduction line, in particular for vacuum-technical apparatus, for example electrical light sources, the current introduction line serving to conduct the electrical current through a glass-like material and forming a hermetic seal with the glass-like material and furthermore the current introduction line consisting of molybdenum and at least on which the glass-like material comes into contact with the surface is provided with a metallic coating, which according to the invention consists of a rhenium layer.

Es wurde festgestellt, daß die Dicke der Rheniumschicht im Hinblick auf die Lösung der gestellten Aufgabe kein kritischer Faktor ist und daß eine Rhenium schicht von extrem geringer Dicke (Grössenordnung nm,) in überraschender Weise die Schweißbarkeit erheblich erleichtert. Gleichzeitig damit haften glasartige Materialien aller Art, sogar auch das Quarzglas - welches in dieser Hinsicht die meisten Schwierigkeiten verursacht -, daran ausgezeichnet. Es ist daher zweckmäßig die Dicke der Rheniumschicht im Bereich zwischen 3 nm und 1000 nm zu wählen, insbesondere zwischen 10 und 100 nm.It was found that the thickness of the rhenium layer is not a critical factor with regard to the solution of the task and that a rhenium layer of extremely small thickness (order of magnitude nm,) surprisingly considerably facilitates the weldability. At the same time, all kinds of glass-like materials, even quartz glass - which causes the most difficulties in this regard - adhere to it excellently. It is therefore advisable to choose the thickness of the rhenium layer in the range between 3 nm and 1000 nm, in particular between 10 and 100 nm.

Zur Herstellung einer Rheniumschicht sind mehrere Möglichkeiten gegeben, wobei für des Trägermetall aus Molybdän sich als vorteilhaftestes einfachstes Herstellungsverfahren elektrolytische Abscheidung - zweckmässigerweise aus einem Elektrolyte in wäßriger Lösung - erwies.There are several options for producing a rhenium layer, with electrolytic deposition - expediently from an electrolyte in aqueous solution - having proven to be the most advantageous simplest production method for the carrier metal made of molybdenum.

Zur elektrolytischen Abscheidung von Rhenium in wäßriger Lösung sind zahlreiche Verfahren bekannt. Das älteste und, nach Erfahrung der Anmelderin, einfachste Verfahren stellt die Abscheidung aus einer mit Schwefelsäure gesäuerten Lösung von Kalium-Perrhenat dar. Da das Molybdän-Trägermetall im Laufe seiner Herstellung im allgemeinen sowieso einer Bearbeitung elektrochemischer Art ausgesetzt wird (wie z. B. bei Folien, bei denen die seitlichen Ränder durch elektrochemische Abtragung messerschneideartig ausgebildet werden, oder bei Drähten, bei denen das als Schmiermittel verwendete Graphit entfernt wird) kann das kontinuierliche Auftragen der Rheniumschicht dem Herstellungsvorgang einfach angepasst werden. Die elektrolytische Abscheidung ist auf jeden Fall kostengünstig, d. h. im Vergleich mit z. B. der Vakuumverdampfung ein Arbeitsverfahren vom geringen Investitionsbedarf und verhältnismässig geringen Materialverlust.Numerous processes are known for the electrolytic deposition of rhenium in aqueous solution. The oldest and, according to the experience of the applicant, the simplest method is the deposition from a solution of potassium perrhenate acidified with sulfuric acid. Since the molybdenum carrier metal is generally exposed to processing in the course of its manufacture in an electrochemical manner anyway (such as in the case of foils in which the lateral edges are formed in the manner of a knife-edge by electrochemical removal, or in the case of wires in which the graphite used as a lubricant is removed), the continuous application of the rhenium layer can easily be adapted to the production process. Electrolytic deposition is definitely inexpensive, i. H. compared with z. B. vacuum evaporation is a working method of low investment and relatively little loss of material.

Gegenüber dem Rhenium ist es bis zum heutigen Tage nicht gelungen, die elektrolytische Abscheidung des Tantals in wäßriger Lösung zu ermöglichen.Compared to rhenium, it has not been possible to date to enable the electrolytic deposition of tantalum in aqueous solution.

Die Dicke der Rheniumschicht ist, wie erwähnt, kein kritischer Faktor (obwohl dieser unter elektrolytischer Abscheidung gut kontrollierbar ist).As mentioned, the thickness of the rhenium layer is not a critical factor (although this can be controlled well by electrodeposition).

Weist das Molybdän-Trägermetall Folienform auf und muß lediglich die zu verschweißende Seite mit Rhenium überzogen werden, wird die Seite der Überfläche des in den Elektrolyt eintauchenden Molybdän-Trägermetalls die gegenüber dem zu verschweißenden Bereich liegt und mit Rhenium nicht überzogen werden soll, auf einer aus Isolierstoff gefertigten oder mit Isolierstoff verkleideten Stütze, zweckmässigerweise auf einer Walzenfläche geführt.If the molybdenum base metal has a foil shape and only the side to be welded has to be coated with rhenium, the side of the surface of the molybdenum base metal immersed in the electrolyte which lies opposite the area to be welded and should not be coated with rhenium is made out of one Support made or insulated with insulating material, expediently guided on a roller surface.

Beispielweise wird nachfolgend das Überziehen der für die Quarz-Glühkörper von Quecksilberlampen als Trägermetall der Stromeinführungsleitung verwendeten Molybdänfolie mit einer Rheniumschicht beschrieben. Die Folie ist 8,5 mm breit und 25 Jlm dick und ihre Kanten wurden - in an sich bekannter Art und Weise - durch elektrolytische Ätzung messerschneideartig verdünnt. Diese Folie passiert denn eine Metallrolle und anschließend die untere Mantelfläche einer aus lsolierstoff hergestellten oder mit Isolierstoff, wie zum Beispiel mit Gummi, überzogenen Drehwalze mit einem Durchmesser von 100 mm. Die Walze taucht etwa 35 mm tief in den Elektrolyten ein 10 g KRe04 und 4 g konzentrierte H2S04 in 1 Liter Wasser gelöst enthält. Die Gegenelektrode besteht aus Platin und wird an die positive Klemme der Stromquelle angeschlossen. Die negative Klemme der Stromquelle steht mit der Metallwalze, die die Folie vor dem Eintauchen in den Elektrolyten passierte in Verbindung. Die Geschwindigkeit des Vorwärtstransportes der Folie ist so gewählt, dass die Aufenthaltsdauer der betreffenden Stelle der Folie im Elektrolyten etwa 30 Sek. beträgt. Die elektrolytische Abscheidung sollte unter Zimmertemperatur, bei einer Stromdichte von etwa 800 A/m2 ausgeführt werden. Die aus der Elektrolysewanne austretende Folie passiert eine Waschanlage mit Wassergegenstrom, dann eine Trockner mit einer Luftströmung sowie einen laufend mit Wasserstoff gespülten Durchzugsofen mit einer Temperatur von 1100° C. Mittels der beschriebenen Anordnung wird erreicht, daß nur die eine Seite der Folie mit Rhenium überzogen wird. Dies ist jedoch vollkommen ausreichend, da bei der vorliegenden Anwendung nur an einer Seite der Folie die Anschweißung erfolgt. Sollten die beiden Seite oder der Draht überzogen werden, könnte dies ohne weiteres mit den an sich bekannten Verfahren gelöst werden. Die Bedingungen für die elektrolytische Abscheidung können in weiten Grenzen geändert werden.For example, the covering of the molybdenum foil used for the quartz incandescent bodies of mercury lamps as the carrier metal of the power lead is described with a rhenium layer. The film is 8.5 mm wide and 25 J lm thick and its edges - in a manner known per se - were thinned like knife edges by electrolytic etching. This film then passes through a metal roller and then the lower lateral surface of a rotary roller with a diameter of 100 mm, which is made of insulating material or covered with insulating material, such as rubber. The roller dips about 35 mm deep in the electrolyte and contains 10 g of KRe0 4 and 4 g of concentrated H 2 S0 4 dissolved in 1 liter of water. The counter electrode is made of platinum and is connected to the positive terminal of the power source. The negative terminal of the power source is connected to the metal roller that passed the film before immersing it in the electrolyte. The speed of the forward transport of the film is selected so that the duration of the relevant point of the film in the electrolyte is about 30 seconds. The electrolytic deposition should be carried out at room temperature, with a current density of about 800 A / m 2 . The film emerging from the electrolysis bath passes through a washing system Water countercurrent, then a dryer with an air flow and a continuous furnace flushed with hydrogen at a temperature of 1100 ° C. By means of the described arrangement it is achieved that only one side of the film is coated with rhenium. However, this is completely sufficient since, in the present application, the welding takes place only on one side of the film. Should the two sides or the wire be covered, this could easily be solved with the methods known per se. The conditions for electrolytic deposition can be changed within wide limits.

Ferner können Bäder mit einer Zusammensetzung, die von dem Bekannten abweicht, ebenso zur Anwendung kommen.Furthermore, baths with a composition that differs from the known can also be used.

An Stelle der elektrolytischen Abscheidung können auch andere Verfahren zur Ausbildung eines Überzugs zur Anwendung kommen, wie z. B. die Vakuumverdampfung, die Zerstäubung und die chemische Abscheidung aus der Dampfphase (CDV), die jedoch mit erheblichen Mehrkosten und Verlusten verbunden sind.Instead of electrolytic deposition, other methods of forming a coating can also be used, such as. B. vacuum evaporation, atomization and chemical vapor deposition (CDV), which are associated with considerable additional costs and losses.

Die Vorteile der erfindungsgemässen Stromeinführungsleitung bestehen zusammenfassend darin, daß diese besonders gut schweißbar ist, gleichzeitig die hermetische Verbindung mit dem glasaritgen Material bzw. Werkstoff sichert, die Wärmebehandlung im Desoxidationsmedium, wie z. B. im Wasserstoff gut erträgt und neben diesen Vorteilen noch durch ein verhältnismässig preiswertes und einfaches Verfahren hergestellt werden kann.The advantages of the current introduction line according to the invention consist in the fact that it can be welded particularly well, at the same time ensures the hermetic connection with the glass material, the heat treatment in the deoxidation medium, such as, for. B. well endured in hydrogen and besides these advantages can still be produced by a relatively inexpensive and simple process.

Claims (6)

1. Current lead-in line, especially for vacuum technology apparatus, such as, for example, electric light sources, the current lead-in line serving to carry the electric current through a vitreous material and forming a hermetic seal with the vitreous material, and the current lead-in line consisting of molybdenum and being provided with a metal coating, at least on the surface coming into contact with the vitreous material, characterised in that the metal coating consisting of a layer of rhenium.
2. Current lead-in line according to claim 1, characterised in that the rhenium layer has a thickness of between 3 and 1000 nm.
3. Current lead-in line according to claim 1, characterised in that the rhenium layer has a thickness of between 10 and 1000 nm.
4. Process for the manufacture of a current lead-in line that consists of molybdenum and is provided with a metal coating, according to any one of claims 1 to 3, characterised in that the coating, which consists of rhenium, is applied to the molybdenum by electrolytic deposition.
5. Process according to claim 4, characterised in that the electrolytic deposition is effected from an electrolyte in aqueous solution.
6. Process according to claim 4 or 5, characterised in that the current lead-in line consists of a foil, and the foil is guided on a support that is made of insulating material or is covered with insulating material, especially on a roller surface, so that one side of the foil is coated with rhenium by being dipped into the electrolyte.
EP83900433A 1982-01-28 1983-01-27 Power supply conductor, essentially for vacuum apparatus, and manufacturing method thereof Expired EP0098858B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
HU25482 1982-01-28
HU82254A HU185198B (en) 1982-01-28 1982-01-28 Current inlet particularly for vacuumtechnical devices

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EP0098858A1 EP0098858A1 (en) 1984-01-25
EP0098858A4 EP0098858A4 (en) 1984-07-03
EP0098858B1 true EP0098858B1 (en) 1988-05-18

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EP (1) EP0098858B1 (en)
JP (1) JPS59500070A (en)
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DE (1) DE3376709D1 (en)
HU (1) HU185198B (en)
WO (1) WO1983002684A1 (en)

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EP2086002A3 (en) 2004-09-30 2009-10-28 Koninklijke Philips Electronics N.V. Electric lamp with sealing foil

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DE3376709D1 (en) 1988-06-23
EP0098858A4 (en) 1984-07-03
EP0098858A1 (en) 1984-01-25
AT379711B (en) 1986-02-25
US4559278A (en) 1985-12-17
WO1983002684A1 (en) 1983-08-04
ATA7883A (en) 1985-06-15
HU185198B (en) 1984-12-28
JPS59500070A (en) 1984-01-12

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