EP0876670B1 - Method of producing a shaped part from a silver-based contact material - Google Patents

Method of producing a shaped part from a silver-based contact material Download PDF

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Publication number
EP0876670B1
EP0876670B1 EP97914051A EP97914051A EP0876670B1 EP 0876670 B1 EP0876670 B1 EP 0876670B1 EP 97914051 A EP97914051 A EP 97914051A EP 97914051 A EP97914051 A EP 97914051A EP 0876670 B1 EP0876670 B1 EP 0876670B1
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EP
European Patent Office
Prior art keywords
silver
contact material
metal oxide
iron
rhenium
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EP97914051A
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German (de)
French (fr)
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EP0876670A2 (en
Inventor
Franz Hauner
Günter Tiefel
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Metaux Precieux Metalor SA
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METAUX PRECIEUX
Metaux Precieux Metalor SA
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Publication of EP0876670A2 publication Critical patent/EP0876670A2/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/023—Composite material having a noble metal as the basic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/023—Composite material having a noble metal as the basic material
    • H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
    • H01H2001/02378—Composite material having a noble metal as the basic material and containing oxides containing iron-oxide as major component

Definitions

  • the invention relates to a method for producing a Fitting made of a silver-based contact material.
  • the invention further relates to such a contact material as well a fitting made of such a contact material.
  • silver-based contact materials that contain certain active components have long proven themselves. Both metals and metal oxides are known as active components which have a favorable influence on the switching properties of the contact material.
  • Representatives of the silver-based metallic contact materials are, for example, silver-nickel (AgNi) and silver-iron (AgFe). Silver-iron oxide (AgFe 2 O 3 ) may be mentioned as a representative of the oxidic contact materials.
  • Silver-nickel contact materials in particular have good ones Switching properties, but it is disadvantageous that the during manufacture or during operation due to abrasion Nickel dust as well as that which forms as a switching product Nickel oxide has a harmful effect on human Organism.
  • EP 0 586 411 B1 which describes the closest prior art, is a silver-based contact material known that the metals iron and rhenium in mass fractions between 1% and 50% or between 0.01% and 5% contains as active components. It was found that rhenium even in proportions below 1% the properties of a improved such contact material.
  • the contact material mentioned is characterized by low contact heating with stable heating behavior, reasonable tendency to weld and long service life in relation to specified Switching currents.
  • the silver-iron-rhenium contact material by mixing silver and iron-rhenium alloy powder or by mixing separate powders Made of silver, iron and rhenium.
  • the powder mixture is then by compression molding or extrusion as well Sintering into molded parts or semi-finished products.
  • the structure of such a material i.e. the size and distribution of the active components in the silver matrix is through the grain size of the metal powder or alloy powder available on the market specified.
  • the use of coarse metal powders leads to a coarse-grained, fine-grained metal powder to a fine-grained structure.
  • the finest, in technical relevant quantities of iron powder produced have a average grain size of approx. 5 ⁇ m.
  • the powder mixture by compression molding to a molded part, which by sintering and possibly further pressing to a finished one Fitting is processed.
  • the molded part can additionally with a layer of pure silver for a secure connection the contact piece with the base pressed by brazing become.
  • the active components added in powder form are more uniform Grain size irregularly distributed over the silver matrix in front.
  • the structure of the fitting is largely isotropic.
  • the powder mixture is initially too a porous compact or slug is pressed and / or sintered.
  • the compact or slug is, if necessary, with a Layer of pure silver (see above), by extrusion into one Extruded from which the shaped pieces are separated and possibly undergo a subsequent treatment.
  • the structure of the contact material makes its electrical Switching properties, e.g. Erosion, contact resistance and welding power, significantly determined.
  • WO 95/08833 A1 describes a method for connecting a Contact piece made of a silver metal oxide material with a Carrier described by brazing or welding. there the metal oxide becomes in the area of the contact piece near the surface of the contact material at least partially to metal reduced. A resulting, the switching properties the contact piece or the contact material cheap influencing structural change is not achieved.
  • the method described is only suitable for production thin, weldable and solderable layers up to a few 100 ⁇ m.
  • the object of the invention is to provide a manufacturing method for a fitting made of a contact material and such Kunststoffwerkatoff indicate which of the Prior art has more favorable switching properties. It is also an object of the invention to provide a contact piece from the Specify contact material, which improved by Switching properties especially for a switching device in energy technology suitable.
  • This task is related to the manufacturing process a fitting made of a silver-based contact material solved according to the invention by a powder mixture of silver and is formed from a metal oxide, which is powder metallurgy is processed into the molding, and wherein the metal oxide is reduced to metal.
  • the invention is based on the knowledge that a contact material with a fine structure a better switching behavior as a contact material with a coarse structure.
  • the range of properties of a contact material leaves improve significantly by changing the average grain size of the Active components in the silver matrix is reduced.
  • metal oxide powders are available, their grain sizes are significantly smaller than 1 ⁇ m can be used of metal oxide powder instead of metal powder and subsequent Achieve a contact material by reducing the metal oxide, where the average grain size of the metallic active components is in the nanometer range.
  • metal oxide powders under less stringent transportation and processing instructions are worked on, as in In contrast to metal oxide powders, many metal powders are self-igniting are. In this way, the manufacturing costs to reduce.
  • the reduction of the metal oxide is advantageously carried out in the powder mixture, because of the increasing compression of the A complete powder mixture in subsequent steps Reduction of the metal oxide is difficult.
  • the reduction of the metal oxide can also be in a blank of the Molding take place, which still has a sufficiently high porosity or has gas permeability.
  • a blank is for example the one to be made available in extrusion technology Slug, which is subsequently pressed into a strand.
  • Such a blank can also be used in molding technology be produced preliminary product for a molded part before it the molded part is produced by pressing and sintering again becomes.
  • the reduction of the metal oxide is expediently carried out by achieved a heat treatment in a reducing atmosphere. It is particularly effective when the heat treatment in a temperature range of 500 ° C below the melting point of silver, i.e. taking into account the admixed Active components at a temperature between 500 ° C up to 1000 ° C, preferably at 700 ° C, is carried out.
  • the reducing atmosphere as a protective gas used for any sintering that may be required become. Sintering and reduction can thereby occur during production of the contact material can be done in one operation.
  • the gas hydrogen (H 2 ) usually used for the sintering is advantageously also used as the reducing atmosphere.
  • the active component supplied in powder form. This is particularly the case if the active component is in the form of a Powder of a metal oxide with very small grain sizes supplied becomes.
  • the active component can be achieved in the contact material, if as a metal oxide a powder with a grain size of smaller than 1 ⁇ m, preferably from 100 to 500 nm.
  • the manufactured contact material or the molding from the Contact material has advantageous switching properties if the powder mixture is another metal or another Metal oxide is added.
  • the further metal oxide reduced to another metal as described. It but it is also conceivable that the further metal oxide only after to reduce the reduction of the powder mixture.
  • the manufactured one In this case, the contact material would have an oxidic Active component.
  • the powder mixture is silver (Ag), iron oxide (Fe 2 O 3 / Fe 3 O 4 ) and rhenium (Re) or silver (Ag), rhenium oxide (Re) and iron (Fe) or silver (Ag) , Rhenium oxide (ReO) and iron oxide (Fe 2 O 3 / Fe 3 O 4 ) is supplied.
  • the object is achieved according to the invention solved with a contact material based on silver at least one further metallic component, the middle one Grain size is less than 1 micron, preferably 100 to Is 500 nm.
  • a contact material also has very good switching properties, in particular a very low one Welding tendency and a long service life.
  • the contact material has favorable switching properties, if as metallic active components iron (Fe) and rhenium (Re) are provided. It is advantageous if iron (Fe) in mass proportions between 1 and 50% and rhenium (Re) in mass proportions between 0.01 and 5%.
  • the task regarding the contact piece is invented solved by a fitting made of the contact material in shape a contact piece.
  • the contact piece can additionally with a layer of pure silver for a secure connection of the contact piece with the base by brazing be provided.
  • Such a contact piece is suitable for the use in a switching device of energy technology, in particular for a low voltage switch.
  • a silver-iron-rhenium material is produced.
  • silver powder Ag is mixed with rhenium powder Re (grain size approx. 5 ⁇ m) and with iron oxide powder Fe 2 O 3 / Fe 3 O 4 (grain size smaller than 10 nm).
  • This powder mixture is processed into a blank or slug, which is annealed at a temperature of 700 ° C under an H 2 atmosphere to reduce the iron oxide to iron.
  • the further processing into a contact piece takes place according to the extrusion technique described under known conditions.
  • the composition of the powder mixture is such that the Sum of the mass fractions of the active components iron (Fe) and Rhenium (Re) is 8.8% in the finished material Ratio of iron to rhenium 19/1 is chosen.
  • the material is referred to below as Ag (FeRe 95/5) 8.8 be, the indication of the ratio 95/5 on the Mixing ratio of iron and Rhenium powder.
  • Figures 1 and 3 show the fine structure of a manufactured in this way Ag (FeRe 95/5) 8.8 material parallel or vertical to the extrusion direction.
  • the average grain size of the rhenium and iron particles in the silver matrix lies in an area well below 1 ⁇ m.
  • a conventional one manufactured Ag (FeRe 95/5) 8.8 material its structure shown perpendicular to the extrusion direction in Fig. 2 is the size difference is that embedded in the silver matrix Active components significant. So will this 3 and 4 show the structure of the invention or conventionally produced Ag (FeRe 95/5) Show 8.8 material parallel to the direction of extrusion.
  • the welding force values are shown in their total frequency, the ordinate after the Weibull function and the Abscissa is logarithmically divided. As with AgFeRe contact materials the mechanical during the first switching operations Machining can be the cause of high welding power Comparison with conventionally manufactured AgFeRe materials the 99.8% value was used.
  • This result means a 55% improvement in welding behavior of the AgFeRe contact material produced according to the invention compared to a conventionally manufactured one.

Abstract

The invention concerns the production of a shaped part from a silver-based contact material. According to the invention, a powder mixture is formed from silver and a metal oxide and is processed powder-metallurgically to form the shaped part, the metal oxide being reduced to metal. Since metal oxide powders with a considerably finer grain size than metal powders are available, a contact material of which the metal incorporated as active component has an average grain size of less than 1 νm can be obtained. Owing to the fine grain size, a contact material of this type has particularly advantageous switching properties.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung eines Formstücks aus einem Kontaktwerkstoff auf Silberbasis. Die Erfindung betrifft weiter einen solchen Kontaktwerkstoff sowie ein Formstück aus einem solchen Kontaktwerkstoff.The invention relates to a method for producing a Fitting made of a silver-based contact material. The The invention further relates to such a contact material as well a fitting made of such a contact material.

Für ein Kontaktstück in einem Niederspannungs-Schaltgerät der Energietechnik, z.B. in einem Leistungsschalter oder in einem Hilfsschütz, haben sich Kontaktwerkstoffe auf Silberbasis, die bestimmte Wirkkomponenten enthalten, seit langem bewährt. Als Wirkkomponenten, welche die Schalteigenschaften des Kontaktwerkstoffes günstig beeinflussen, sind sowohl Metalle als auch Metalloxide bekannt. Vertreter der metallischen Kontaktwerkstoffe auf Silberbasis sind beispielsweise Silber-Nickel (AgNi) und Silber-Eisen (AgFe). Als Vertreter der oxidischen Kontaktwerkstoffe sei beispielhaft Silber-Eisenoxid (AgFe2O3) genannt.For a contact piece in a low-voltage switchgear in power engineering, for example in a circuit breaker or in an auxiliary contactor, silver-based contact materials that contain certain active components have long proven themselves. Both metals and metal oxides are known as active components which have a favorable influence on the switching properties of the contact material. Representatives of the silver-based metallic contact materials are, for example, silver-nickel (AgNi) and silver-iron (AgFe). Silver-iron oxide (AgFe 2 O 3 ) may be mentioned as a representative of the oxidic contact materials.

Während oxidische Kontaktwerkstoffe gegenüber metallischen Kontaktwerkstoffen eine geringere Verschweißneigung aufweisen, besitzen letztgenannte insbesondere bei kleinen Strömen eine höhere Lebensdauer.While oxidic contact materials versus metallic Contact materials have a lower tendency to weld, possess the latter especially with small currents a longer lifespan.

Zur Messung bestimmter Eigenschaften eines Kontaktwerktoffes wird üblicherweise ein in Z. f. Werkstofftechnik/J. of Materials Technology 7, (1976), 381 bis 389 beschriebener Prüfschalter herangezogen, in den jeweils ein Kontaktstück aus dem Kontaktwerkstoff eingesetzt wird.For measuring certain properties of a contact material is usually a in Z. f. Materials Engineering / J. of materials Technology 7, (1976), 381 to 389 test switch described used, in each of which a contact piece the contact material is used.

Besonders Silber-Nickel-Kontaktwerkstoffe besitzen gute Schalteigenschaften, jedoch ist nachteilig, daß der sich bei der Herstellung oder während des Betriebs durch Abrieb bildende Nickelstaub sowie das sich als Schaltprodukt bildende Nickeloxid eine schädliche Auswirkung auf den menschlichen Organismus haben kann.Silver-nickel contact materials in particular have good ones Switching properties, but it is disadvantageous that the during manufacture or during operation due to abrasion Nickel dust as well as that which forms as a switching product Nickel oxide has a harmful effect on human Organism.

Aus der EP 0 586 411 B1,die den nächstliegenden Stand der Technik beschreibt, ist ein Kontaktwerkstoff auf Silberbasis bekannt, der die Metalle Eisen und Rhenium in Massenanteilen zwischen 1 % und 50 % bzw. zwischen 0,01 % und 5 % als Wirkkomponenten enthält. Dabei wurde erkannt, daß Rhenium selbst in Massenanteilen unter 1 % die Eigenschaften eines derartigen Kontaktwerkstoffes verbessert. Der genannte Kontaktwerkstoff zeichnet sich durch eine geringe Kontakterwärmung mit stabilem Erwärmungsverhalten, vertretbare Verschweißneigung und hohe Lebensdauer in bezug auf vorgegebene Schaltstromstärken aus.EP 0 586 411 B1, which describes the closest prior art, is a silver-based contact material known that the metals iron and rhenium in mass fractions between 1% and 50% or between 0.01% and 5% contains as active components. It was found that rhenium even in proportions below 1% the properties of a improved such contact material. The contact material mentioned is characterized by low contact heating with stable heating behavior, reasonable tendency to weld and long service life in relation to specified Switching currents.

Gemäß der EP 0 586 411 B1 wird der Silber-Eisen-Rhenium-Kontaktwerkstoff durch Mischen von Silber- und Eisen-Rhenium-Legierungspulver oder durch Mischen von separaten Pulvern aus Silber, Eisen und Rhenium hergestellt. Die Pulvermischung wird anschließend durch Formpressen oder Strangpressen sowie Sintern zu Formteilen bzw. zu Halbzeugen verarbeitet. Das Gefüge eines solchen Werkstoffes, d.h. die Größe und die Verteilung der Wirkkomponenten in der Silbermatrix, ist durch die Korngröße der am Markt erhältlichen Metallpulver bzw. Legierungspulver vorgegeben. Die Verwendung von groben Metallpulvern führt zu einem grobkörnigen, von feinkörnigen Metallpulvern zu einem feinkörnigen Gefüge. Die feinsten, in technisch relevanten Mengen hergestellten Eisen-Pulver haben eine mittlere Korngröße von ca. 5 µm. Eisen-Rhenium-Pulver werden durch Verdüsen einer entsprechenden Schmelze hergestellt und besitzen ebenfalls eine mittlere Korngröße von ca. 5 µm oder mehr.According to EP 0 586 411 B1, the silver-iron-rhenium contact material by mixing silver and iron-rhenium alloy powder or by mixing separate powders Made of silver, iron and rhenium. The powder mixture is then by compression molding or extrusion as well Sintering into molded parts or semi-finished products. The structure of such a material, i.e. the size and distribution of the active components in the silver matrix is through the grain size of the metal powder or alloy powder available on the market specified. The use of coarse metal powders leads to a coarse-grained, fine-grained metal powder to a fine-grained structure. The finest, in technical relevant quantities of iron powder produced have a average grain size of approx. 5 µm. Be iron rhenium powder produced by atomizing a corresponding melt and also have an average grain size of approx. 5 µm or more.

Zur Herstellung eines Formstücks aus dem Kontaktwerkstoff sind im wesentlichen zwei verschiedene pulvermetallurgische Verfahren bekannt. Bei der Formteiltechnik wird die Pulvermischung durch Formpressen zu einem Formteil verpreßt, welches durch Sintern und ggf. weiteres Pressen zu einem fertigen Formstück verarbeitet wird. Für die Herstellung eines Formstücks in Form eines Kontaktstücks kann das Formteil zusätzlich mit einer Schicht aus Reinsilber zur sicheren Verbindung des Kontaktstücks mit der Unterlage durch Hartlöten verpreßt werden.For the production of a molded part from the contact material are essentially two different powder metallurgical Process known. In molding technology, the powder mixture by compression molding to a molded part, which by sintering and possibly further pressing to a finished one Fitting is processed. For the production of a fitting in the form of a contact piece, the molded part can additionally with a layer of pure silver for a secure connection the contact piece with the base pressed by brazing become.

In einem nach der Formteiltechnik hergestellten Formstück liegen die in Pulverform zugefügten Wirkkomponenten mit einheitlicher Korngröße unregelmäßig über die Silbermatrix verteilt vor. Das Gefüge des Formstücks ist weitgehend isotrop.In a molded part manufactured using molding technology the active components added in powder form are more uniform Grain size irregularly distributed over the silver matrix in front. The structure of the fitting is largely isotropic.

Bei der Strangpreßtechnik wird die Pulvermischung zunächst zu einem porösen Preßling oder Butzen gepreßt und/oder gesintert. Der Preßling oder Butzen wird, gegebenenfalls mit einer Schicht aus Reinsilber (s.o.), durch Strangpressen zu einem Strang verpreßt, aus welchem die Formstücke abgetrennt und eventuell einer nachfolgenden Behandlung unterzogen werden.In the extrusion technique, the powder mixture is initially too a porous compact or slug is pressed and / or sintered. The compact or slug is, if necessary, with a Layer of pure silver (see above), by extrusion into one Extruded from which the shaped pieces are separated and possibly undergo a subsequent treatment.

In einem nach der Strangpreßtechnik hergestellten Formstück sind die Pulverkörner des Silbers und ggf. der Wirkkomponenten in Strangpreßrichtung verformt bzw. ausgerichtet, wodurch sich ein anisotropes, nämlich zeiliges Gefüge ausbildet.In a fitting manufactured using the extrusion technique are the powder grains of silver and possibly the active components deformed or aligned in the extrusion direction, whereby an anisotropic, namely line structure is formed.

Durch das Gefüge des Kontaktwerkstoffs werden seine elektrischen Schalteigenschaften, z.B. Abbrand, Kontaktwiderstand und Schweißkraft, maßgeblich bestimmt.The structure of the contact material makes its electrical Switching properties, e.g. Erosion, contact resistance and welding power, significantly determined.

In der WO 95/08833 A1 wird ein Verfahren zum Verbinden eines Kontaktstückes aus einem Silber-Metalloxid-Werkstoff mit einem Träger durch Hartlöten oder Schweißen beschrieben. Dabei wird im oberflächennahen Bereich des Kontaktstückes das Metalloxid des Kontaktwerkstoffes wenigstens teilweise zu Metall reduziert. Eine daraus resultierende, die Schalteigenschaften des Kontaktstückes bzw. des Kontaktwerkstoffes günstig beeinflussende Gefügeveränderung wird nicht erreicht. Das beschriebene Verfahren eignet sich lediglich zur Herstellung dünner, schweiß- und lötbarer Schichten bis zu wenigen 100 µm.WO 95/08833 A1 describes a method for connecting a Contact piece made of a silver metal oxide material with a Carrier described by brazing or welding. there the metal oxide becomes in the area of the contact piece near the surface of the contact material at least partially to metal reduced. A resulting, the switching properties the contact piece or the contact material cheap influencing structural change is not achieved. The method described is only suitable for production thin, weldable and solderable layers up to a few 100 µm.

Aufgabe der Erfindung ist es, ein Herstellungsverfahren für ein Formstück aus einem Kontaktwerkstoff sowie einen solchen Kontaktwerkatoff selbst anzugeben, welcher gegenüber dem Stand der Technik günstigere Schalteigenschaften aufweist. Ferner ist es Aufgabe der Erfindung, ein Kontaktstück aus dem Kontaktwerkstoff anzugeben, welches sich durch verbesserte Schalteigenschaften besonders für ein Schaltgerät der Energietechnik eignet.The object of the invention is to provide a manufacturing method for a fitting made of a contact material and such Kontaktwerkatoff indicate which of the Prior art has more favorable switching properties. It is also an object of the invention to provide a contact piece from the Specify contact material, which improved by Switching properties especially for a switching device in energy technology suitable.

Diese Aufgabe wird bezüglich des Verfahrens zur Herstellung eines Formstücks aus einem Kontaktwerkstoff auf Silberbasis erfindungsgemäß gelöst, indem eine Pulvermischung aus Silber und aus einem Metalloxid gebildet wird, welche pulvermetallurgisch zu dem Formstück verarbeitet wird, und wobei das Metalloxid zu Metall reduziert wird.This task is related to the manufacturing process a fitting made of a silver-based contact material solved according to the invention by a powder mixture of silver and is formed from a metal oxide, which is powder metallurgy is processed into the molding, and wherein the metal oxide is reduced to metal.

Die Erfindung geht dabei von der Erkenntnis aus, daß ein Kontaktwerkstoff mit einem feinen Gefüge ein besseres Schaltverhalten als ein Kontaktwerkstoff mit einem groben Gefüge aufweist. Das Eigenschaftsspektrum eines Kontaktwerkstoffes laßt sich erheblich verbessern, indem die mittlere Korngröße der Wirkkomponenten in der Silbermatrix verringert wird.The invention is based on the knowledge that a contact material with a fine structure a better switching behavior as a contact material with a coarse structure. The range of properties of a contact material leaves improve significantly by changing the average grain size of the Active components in the silver matrix is reduced.

Umfangreiche Messungen lassen erwarten, daß die Schalteigenschaften eines Kontaktwerkstoffes auf Silberbasis bzw. die Schalteigenschaften eines Formstücks aus dem Kontaktwerkstoff besonders günstig sind, falls die mittlere Korngröße der Wirkkomponenten kleiner als 1 µm ist. Ein derartiger Kontaktwerkstoff läßt sich mit bekannten pulvermetallurgischen Herstellungsverfahren bei Verwendung handelsüblicher Metallpulver, deren mittlere Korngröße im Bereich einiger µm liegt, allerdings nicht erzeugen. Extensive measurements suggest that the switching properties a silver-based contact material or the Switching properties of a fitting made of the contact material are particularly favorable if the average grain size of the Active components is less than 1 µm. Such a contact material can be done with known powder metallurgical manufacturing processes when using commercially available metal powder, whose average grain size is in the range of a few µm, but do not generate.

Da jedoch Metalloxid-Pulver verfügbar sind, deren Korngrößen wesentlich kleiner als 1 µm sind, läßt sich durch die Verwendung von Metalloxid-Pulver statt Metall-Pulver und anschließende Reduktion des Metalloxids ein Kontaktwerkstoff erzielen, bei dem die mittlere Korngröße der metallischen Wirkkomponenten im Nanometer-Bereich liegt. Zudem kann bei der Verwendung von Metalloxid-Pulvern unter weniger strengen Transport- und Verarbeitungsvorschriften gearbeitet werden, da im Gegensatz zu Metalloxid-Pulvern viele Metall-Pulver selbstentzündlich sind. Auf diese Weise lassen sich die Herstellungskosten reduzieren.However, since metal oxide powders are available, their grain sizes are significantly smaller than 1 µm can be used of metal oxide powder instead of metal powder and subsequent Achieve a contact material by reducing the metal oxide, where the average grain size of the metallic active components is in the nanometer range. In addition, when using of metal oxide powders under less stringent transportation and processing instructions are worked on, as in In contrast to metal oxide powders, many metal powders are self-igniting are. In this way, the manufacturing costs to reduce.

Die Reduktion des Metalloxides erfolgt vorteilhafterweise in der Pulvermischung, da durch die zunehmende Verdichtung der Pulvermischung in nachfolgenden Arbeitsschritten eine vollständige Reduktion des Metalloxids erschwert ist.The reduction of the metal oxide is advantageously carried out in the powder mixture, because of the increasing compression of the A complete powder mixture in subsequent steps Reduction of the metal oxide is difficult.

Die Reduktion des Metalloxids kann auch in einem Rohling des Formstücks erfolgen, welcher noch eine genügend hohe Porosität bzw. Gasdurchlässigkeit aufweist. Ein solcher Rohling ist beispielsweise der in der Strangpreßtechnik bereitzustellende Butzen, der nachfolgend zu einem Strang verpreßt wird. Ebenso kann ein solcher Rohling aber auch ein in der Formteiltechnik hergestelltes Vorprodukt für ein Formteil sein, ehe aus diesem durch erneutes Pressen und Sintern das Formteil hergestellt wird.The reduction of the metal oxide can also be in a blank of the Molding take place, which still has a sufficiently high porosity or has gas permeability. Such a blank is for example the one to be made available in extrusion technology Slug, which is subsequently pressed into a strand. As well Such a blank can also be used in molding technology be produced preliminary product for a molded part before it the molded part is produced by pressing and sintering again becomes.

Zweckmäßigerweise wird die Reduktion des Metalloxids durch eine Wärmebehandlung in einer reduzierenden Atmosphäre erreicht. Besonders effektiv ist es, wenn die Wärmebehandlung in einem Temperaturbereich von 500 °C unterhalb des Schmelzpunktes von Silber, d.h. unter Berücksichtigung der beigemischten Wirkkomponenten bei einer Temperatur zwischen 500 °C bis 1000 °C, vorzugsweise bei 700 °C, durchgeführt wird. Dabei kann die reduzierende Atmosphäre gleichzeitig als Schutzgas für eine eventuell erforderliche Sinterung herangezogen werden. Sinterung und Reduktion können dadurch bei der Herstellung des Kontaktwerkstoffes in einem Arbeitsgang erfolgen.The reduction of the metal oxide is expediently carried out by achieved a heat treatment in a reducing atmosphere. It is particularly effective when the heat treatment in a temperature range of 500 ° C below the melting point of silver, i.e. taking into account the admixed Active components at a temperature between 500 ° C up to 1000 ° C, preferably at 700 ° C, is carried out. there can use the reducing atmosphere as a protective gas used for any sintering that may be required become. Sintering and reduction can thereby occur during production of the contact material can be done in one operation.

Vorteilhafterweise wird als reduzierende Atmosphäre auch das üblicherweise für die Sinterung eingesetzte Gas Wasserstoff (H2) verwendet.The gas hydrogen (H 2 ) usually used for the sintering is advantageously also used as the reducing atmosphere.

Durch die bei pulvermetallurgischen Herstellungsverfahren notwendigen Sinter- und Preßvorgänge kann es zu einer Konglomeration der in Pulverform zugeführten Wirkkomponente kommen. Dies insbesondere, falls die Wirkkomponente in Form eines Pulvers eines Metalloxids mit sehr kleinen Korngrößen zugeführt wird. Für die Schalteigenschaften günstige Korngrößen der Wirkkomponente lassen sich im Kontaktwerkstoff erzielen, wenn als Metalloxid ein Pulver mit einer Korngröße von kleiner als 1 µm, vorzugsweise von 100 bis 500 nm verwendet wird.Through the powder metallurgical manufacturing process necessary sintering and pressing processes can lead to a conglomeration of the active component supplied in powder form. This is particularly the case if the active component is in the form of a Powder of a metal oxide with very small grain sizes supplied becomes. Favorable grain sizes for the switching properties the active component can be achieved in the contact material, if as a metal oxide a powder with a grain size of smaller than 1 µm, preferably from 100 to 500 nm.

Der hergestellte Kontaktwerkstoff bzw. das Formstück aus dem Kontaktwerkstoff weist vorteilhafte Schalteigenschaften auf, wenn der Pulvermischung ein weiteres Metall oder ein weiteres Metalloxid beigemischt wird. Dabei wird das weitere Metalloxid, wie beschrieben, zu einem weiteren Metall reduziert. Es ist aber auch vorstellbar, das weitere Metalloxid erst nach der Reduktion der Pulvermischung beizumengen. Der hergestellte Kontaktwerkstoff hätte in diesem Fall eine oxidische Wirkkomponente.The manufactured contact material or the molding from the Contact material has advantageous switching properties if the powder mixture is another metal or another Metal oxide is added. The further metal oxide, reduced to another metal as described. It but it is also conceivable that the further metal oxide only after to reduce the reduction of the powder mixture. The manufactured one In this case, the contact material would have an oxidic Active component.

Besonders vorteilhaft ist es, wenn der Pulvermischung Silber (Ag), Eisenoxid (Fe2O3/Fe3O4) und Rhenium (Re) oder Silber (Ag), Rheniumoxid (Re) und Eisen (Fe) oder Silber (Ag), Rheniumoxid (ReO) und Eisenoxid (Fe2O3/Fe3O4) zugeführt wird.It is particularly advantageous if the powder mixture is silver (Ag), iron oxide (Fe 2 O 3 / Fe 3 O 4 ) and rhenium (Re) or silver (Ag), rhenium oxide (Re) and iron (Fe) or silver (Ag) , Rhenium oxide (ReO) and iron oxide (Fe 2 O 3 / Fe 3 O 4 ) is supplied.

Bezüglich des Kontaktwerkstoffes wird die Aufgabe erfindungsgemäß gelöst durch einen Kontaktwerkstoff auf Silberbasis mit zumindest einer weiteren metallischen Komponente, deren mittlere Korngröße kleiner als 1 µm ist, vorzugsweise 100 bis 500 nm beträgt. Ein derartiger Kontaktwerkstoff weist neben sehr guten Schalteigenschaften insbesondere eine sehr geringe Verschweißneigung sowie eine hohe Lebensdauer auf.With regard to the contact material, the object is achieved according to the invention solved with a contact material based on silver at least one further metallic component, the middle one Grain size is less than 1 micron, preferably 100 to Is 500 nm. Such a contact material also has very good switching properties, in particular a very low one Welding tendency and a long service life.

Günstige Schalteigenschaften besitzt der Kontaktwerkstoff, wenn als metallische Wirkkomponenten Eisen (Fe) und Rhenium (Re) vorgesehen sind. Dabei ist es vorteilhaft, wenn Eisen (Fe) in Massenanteilen zwischen 1 und 50 % und Rhenium (Re) in Massenanteilen zwischen 0,01 und 5 % vorliegen.The contact material has favorable switching properties, if as metallic active components iron (Fe) and rhenium (Re) are provided. It is advantageous if iron (Fe) in mass proportions between 1 and 50% and rhenium (Re) in mass proportions between 0.01 and 5%.

Die Aufgabe bezüglich des Kontaktstücks wird erfindungsgemäß gelöst durch ein Formstück aus dem Kontaktwerkstoff in Gestalt eines Kontaktstückes. Dabei kann das Kontaktstück zusätzlich mit einer Schicht aus Reinsilber zur sicheren Verbindung des Kontaktstücks mit der Unterlage durch Hartlöten versehen sein. Ein derartiges Kontaktstück eignet sich für die Verwendung in einem Schaltgerät der Energietechnik, insbesondere für einen Niederspannungsschalter.The task regarding the contact piece is invented solved by a fitting made of the contact material in shape a contact piece. The contact piece can additionally with a layer of pure silver for a secure connection of the contact piece with the base by brazing be provided. Such a contact piece is suitable for the use in a switching device of energy technology, in particular for a low voltage switch.

Durch die folgenden Untersuchungsergebnisse sowie durch eine Zeichnung wird ein Ausführungsbeispiel der Erfindung näher erläutert.By the following test results as well as by a Drawing is an embodiment of the invention closer explained.

Dabei zeigen:

FIG 1
Gefüge eines erfindungsgemäß nach der Strangpreß-technik hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes senkrecht zur Strangpreßrichtung;
FIG 2
Gefüge eines konventionell nach der Strangpreßtechnik hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes senkrecht zur Strangpreßrichtung;
FIG 3
Gefüge eines erfindungsgemäß nach der Strangpreß-technik hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes parallel zur Strangpreßrichtung;
FIG 4
Gefüge eines konventionell nach der Strangpreßtechnik hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes parallel zur Strangpreßrichtung.
Show:
FIG. 1
Microstructure of an Ag (FeRe 95/5) 8.8 material produced according to the extrusion technology according to the invention perpendicular to the extrusion direction;
FIG 2
Structure of an Ag (FeRe 95/5) 8,8 material conventionally produced by the extrusion technique perpendicular to the extrusion direction;
FIG 3
Microstructure of an Ag (FeRe 95/5) 8.8 material produced according to the extrusion technique according to the invention parallel to the extrusion direction;
FIG 4
Structure of an Ag (FeRe 95/5) 8,8 material conventionally manufactured according to the extrusion technique parallel to the extrusion direction.

Als Ausführungsbeispiel der Erfindung wird ein Silber-Eisen-Rhenium-Werkstoff hergestellt. Dazu wird Silberpulver Ag mit Rheniumpulver Re (Korngröße ca. 5 µm) und mit Eisenoxid-Pulver Fe2O3/Fe3O4 (Korngröße kleiner als 10 nm) vermischt. Dieses Pulvergemisch wird zu einem Rohling oder Butzen weiterverarbeitet, welcher bei einer Temperatur von 700 °C unter einer H2-Atmosphäre zur Reduktion des Eisenoxids zu Eisen geglüht wird. Die Weiterverarbeitung zu einem Kontaktstück geschieht nach der beschriebenen Strangpreßtechnik unter bekannten Bedingungen.As an exemplary embodiment of the invention, a silver-iron-rhenium material is produced. For this purpose, silver powder Ag is mixed with rhenium powder Re (grain size approx. 5 µm) and with iron oxide powder Fe 2 O 3 / Fe 3 O 4 (grain size smaller than 10 nm). This powder mixture is processed into a blank or slug, which is annealed at a temperature of 700 ° C under an H 2 atmosphere to reduce the iron oxide to iron. The further processing into a contact piece takes place according to the extrusion technique described under known conditions.

Die Zusammensetzung der Pulvermischung ist derart, daß die Summe der Massenanteile der Wirkkomponenten Eisen (Fe) und Rhenium (Re) 8,8 % im fertigen Werkstoff beträgt, wobei das Verhältnis von Eisen zu Rhenium 19/1 gewählt ist. Der Werkstoff soll im folgenden mit Ag (FeRe 95/5) 8,8 bezeichnet werden, wobei sich die Angabe des Verhältnisses 95/5 auf das fertigungstechnisch bedingte Mischungsverhältnis von Eisenund Rhenium-Pulver bezieht.The composition of the powder mixture is such that the Sum of the mass fractions of the active components iron (Fe) and Rhenium (Re) is 8.8% in the finished material Ratio of iron to rhenium 19/1 is chosen. The material is referred to below as Ag (FeRe 95/5) 8.8 be, the indication of the ratio 95/5 on the Mixing ratio of iron and Rhenium powder.

Figuren 1 und 3 zeigen die feine Struktur eines derart hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes parallel bzw. senkrecht zur Strangpreßrichtung. Die mittlere Korngröße der Rhenium- und Eisenpartikel in der Silbermatrix (gemessen senkrecht zur Strangpreßrichtung, s Fig. 1) liegt in einem Bereich deutlich unter 1 µm. Im Vergleich zu einem konventionell hergestellten Ag (FeRe 95/5) 8,8-Werkstoff, dessen Gefüge senkrecht zur Strangpreßrichtung in Fig. 2 dargestellt ist, ist der Größenunterschied der in die Silbermatrix eingebetteten Wirkkomponenten signifikant. Ebenso wird dies auch in den Figuren 3 und 4 ersichtlich, die das Gefüge eines erfindungsgemäß bzw. konventionell hergestellten Ag (FeRe 95/5) 8,8-Werkstoffes parallel zur Strangpreßrichtung zeigen. Figures 1 and 3 show the fine structure of a manufactured in this way Ag (FeRe 95/5) 8.8 material parallel or vertical to the extrusion direction. The average grain size of the rhenium and iron particles in the silver matrix (measured vertically to the extrusion direction, see Fig. 1) lies in an area well below 1 µm. Compared to a conventional one manufactured Ag (FeRe 95/5) 8.8 material, its structure shown perpendicular to the extrusion direction in Fig. 2 is the size difference is that embedded in the silver matrix Active components significant. So will this 3 and 4 show the structure of the invention or conventionally produced Ag (FeRe 95/5) Show 8.8 material parallel to the direction of extrusion.

Als ein für das Schaltverhalten des Werkstoffs signifikanter Parameter wird die Schweißkraft des Werkstoffs nach Z. f. Werkstofftechnik/J. of Materials Technology 7, (1976) 381 bis 389 mit folgenden Prüfbedingungen getestet:

  • Probenabmessung: 10 mm x 10 mm
  • Kontaktfläche: ballig R = 80 mm
  • Oberflächenzustand: gedreht
  • Schließgeschwindigkeit: 1 m/sek.
  • Kontaktkraft: 60 N
  • Prellzeit der ersten drei Sprünge: 5 msek.
  • Trenngeschwindigkeit: 7,4 x 10-4 m/sek.
  • Prüfspannung: 220 V
  • Einschalt- und Ausschaltstrom: 1000 A
  • Schaltzahl 1000.
The welding strength of the material according to Z. f. Materials Engineering / J. of Materials Technology 7, (1976) 381 to 389 tested with the following test conditions:
  • Sample dimensions: 10 mm x 10 mm
  • Contact surface: spherical R = 80 mm
  • Surface condition: rotated
  • Closing speed: 1 m / sec.
  • Contact force: 60 N.
  • Bounce time of the first three jumps: 5 msec.
  • Cutting speed: 7.4 x 10 -4 m / sec.
  • Test voltage: 220 V
  • Switch-on and switch-off current: 1000 A.
  • Number of operations 1000.

Die Schweißkraftwerte werden in ihrer Summenhäufigkeit dargestellt, wobei die Ordinate nach der Weibull-Funktion und die Abszisse logarithmisch geteilt ist. Da bei AgFeRe-Kontaktwerkstoffen bei den ersten Schaltvorgängen die mechanische Bearbeitung Ursache hoher Schweißkraft sein kann, wird zum Vergleich mit konventionell hergestellten AgFeRe-Werkstoffen der 99,8 %-Wert herangezogen.The welding force values are shown in their total frequency, the ordinate after the Weibull function and the Abscissa is logarithmically divided. As with AgFeRe contact materials the mechanical during the first switching operations Machining can be the cause of high welding power Comparison with conventionally manufactured AgFeRe materials the 99.8% value was used.

Es ergibt sich:The result is:

Erfindungsgemäßes Verfahren, Ag (FeRe 95/5) 8,8-Werkstoff:

  • Schweißkraft: 237 N (99,8 %)
  • Konventionelles Verfahren, Ag (FeRe 95/5) 8,8-Werkstoff mit groben Gefüge:
  • Schweißkraft: 530 N (99,8 %).
    • Process according to the invention, Ag (FeRe 95/5) 8.8 material:
  • Welding force: 237 N (99.8%)
  • Conventional process, Ag (FeRe 95/5) 8,8 material with rough structure:
  • Welding force: 530 N (99.8%).

    • Dieses Ergebnis bedeutet ein um 55 % verbessertes Schweißverhalten des erfindungsgemäß hergestellen AgFeRe-Kontaktwerkstoffes gegenüber einem konventionell hergestellten.This result means a 55% improvement in welding behavior of the AgFeRe contact material produced according to the invention compared to a conventionally manufactured one.

    Claims (12)

    1. Process for producing a shaped part from a silver-based contact material, in which a powder mixture is formed from silver and a metal oxide, and this powder mixture is processed using powder metallurgy methods to form the shaped part, and the metal oxide being reduced in the powder mixture or in a blank of the shaped part, to form metal.
    2. Process according to Claim 1, characterized in that the reduction of the metal oxide is carried out by a heat treatment in a reducing atmosphere.
    3. Process according to Claim 2, characterized in that the heat treatment is carried out at a temperature of 500 to 1000°C, preferably at 700°C.
    4. Process according to one of Claims 2 to 3, characterized in that the reducing atmosphere is hydrogen (H2).
    5. Process according to one of Claims 1 to 4, characterized in that the metal oxide used is a powder with a grain size of less than 1 µm, preferably from 100 to 500 nm.
    6. Process according to one of Claims 1 to 5, characterized in that a further metal or a further metal oxide is admixed with the powder mixture.
    7. Process according to. Claim 6, characterized in that silver (Ag), iron oxide (Fe2O3/Fe3O4) and rhenium (Re) or silver (Ag), rhenium oxide (ReO) and iron or silver (Ag), rhenium oxide (ReO) and iron oxide (Fe2O3/Fe3O4) is fed to the powder mixture.
    8. Silver-based contact material having at least one further component which has been reduced to form metal and the mean grain size of which is less than 1 µm, preferably between 100 and 500 nm.
    9. Contact material according to Claim 8, characterized in that iron (Fe) and/or rhenium (Re) are provided as further metallic components.
    10. Contact material according to Claim 9, characterized in that the proportion by mass of the iron (Fe) is between 1% and 50%, and the proportion by mass of the rhenium (Re) is between 0.01% and 5%.
    11. Shaped part made. from a contact material according to one of Claims 8 to 10.
    12. Shaped part according to Claim 11, which is designed as a contact piece for power-engineering switching equipment, in particular for a low-voltage circuit breaker.
    EP97914051A 1996-01-26 1997-01-13 Method of producing a shaped part from a silver-based contact material Expired - Lifetime EP0876670B1 (en)

    Applications Claiming Priority (3)

    Application Number Priority Date Filing Date Title
    DE19602812 1996-01-26
    DE19602812A DE19602812C1 (en) 1996-01-26 1996-01-26 Method for producing a shaped piece from a silver-based contact material and shaped piece
    PCT/DE1997/000042 WO1997027601A2 (en) 1996-01-26 1997-01-13 Method of producing a shaped part from a silver-based contact material

    Publications (2)

    Publication Number Publication Date
    EP0876670A2 EP0876670A2 (en) 1998-11-11
    EP0876670B1 true EP0876670B1 (en) 2002-05-15

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    EP (1) EP0876670B1 (en)
    JP (1) JPH11503559A (en)
    BR (1) BR9707202B1 (en)
    DE (2) DE19602812C1 (en)
    ES (1) ES2176718T3 (en)
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    JP3825275B2 (en) * 2001-04-13 2006-09-27 株式会社日立製作所 Electrical contact member and its manufacturing method
    CN1820335A (en) * 2004-06-18 2006-08-16 田中贵金属工业株式会社 Relay for sealed AC load and ag-base contact element material for use therein

    Family Cites Families (13)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US2145690A (en) * 1937-09-24 1939-01-31 Mallory & Co Inc P R Electric contact material
    US2664618A (en) * 1944-04-22 1954-01-05 Fansteel Metallurgical Corp Electrical contact
    US3135601A (en) * 1961-11-16 1964-06-02 Martin Marietta Corp Alumina-silver alloy
    US3505065A (en) * 1968-08-12 1970-04-07 Talon Inc Method of making sintered and infiltrated refractory metal electrical contacts
    GB1536847A (en) * 1976-07-12 1978-12-20 Square D Co Electrically conductive composite materials
    GB1524074A (en) * 1976-07-12 1978-09-06 Square D Co Electrically conductive composite materials
    US4361033A (en) * 1979-01-02 1982-11-30 Gte Laboratories Incorporated Method for selecting an additive for electrical contacts
    US5286441A (en) * 1989-12-26 1994-02-15 Akira Shibata Silver-metal oxide composite material and process for producing the same
    DE4117312A1 (en) * 1991-05-27 1992-12-03 Siemens Ag SILVER-BASED CONTACT MATERIAL FOR USE IN SWITCHGEAR DEVICES OF ENERGY TECHNOLOGY AND METHOD FOR THE PRODUCTION OF CONTACT PIECES FROM THIS MATERIAL
    DE4117311A1 (en) * 1991-05-27 1992-12-03 Siemens Ag CONTACT MATERIAL ON A SILVER BASE FOR USE IN SWITCHGEAR DEVICES IN ENERGY TECHNOLOGY
    DE4331913A1 (en) * 1993-09-20 1995-03-23 Siemens Ag Method for connecting a contact pad made of silver-metal oxide material to a metallic contact carrier
    JPH0896643A (en) * 1994-09-28 1996-04-12 Matsushita Electric Works Ltd Electric contact point material
    DE19543223C1 (en) * 1995-11-20 1997-02-20 Degussa Silver@-iron@ material contg. oxide additives

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    WO1997027601A3 (en) 1997-10-09
    ES2176718T3 (en) 2002-12-01
    DE59707280D1 (en) 2002-06-20
    BR9707202A (en) 1999-04-06
    BR9707202B1 (en) 2010-06-29
    WO1997027601A2 (en) 1997-07-31
    US6001149A (en) 1999-12-14
    EP0876670A2 (en) 1998-11-11
    JPH11503559A (en) 1999-03-26
    DE19602812C1 (en) 1997-07-31

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