EP2831298B1 - Matière active composite - Google Patents

Matière active composite Download PDF

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Publication number
EP2831298B1
EP2831298B1 EP13715919.0A EP13715919A EP2831298B1 EP 2831298 B1 EP2831298 B1 EP 2831298B1 EP 13715919 A EP13715919 A EP 13715919A EP 2831298 B1 EP2831298 B1 EP 2831298B1
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EP
European Patent Office
Prior art keywords
contact material
oxide
contact
magnesium
magnesium stannate
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.)
Active
Application number
EP13715919.0A
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German (de)
English (en)
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EP2831298A1 (fr
Inventor
Michael Bender
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Saxonia Technical Materials GmbH
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Saxonia Technical Materials GmbH
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Publication date
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Priority to EP13715919.0A priority Critical patent/EP2831298B1/fr
Publication of EP2831298A1 publication Critical patent/EP2831298A1/fr
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • 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
    • H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
    • H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2

Definitions

  • silver / metal and silver / metal oxide composites have proven themselves.
  • the silver / metal composite most commonly used is silver / nickel, which has its main application at lower currents.
  • the AgSnO 2 WO 3 / MoO 3 material is produced by powder metallurgy using the extrusion technique.
  • the powder metallurgical production has the advantage that additives of any kind and quantity can be used.
  • the material can be specifically optimized for certain properties, such as welding force or heating.
  • the combination of powder metallurgy with the extrusion technology allows a particularly high efficiency in the production of the contact pieces.
  • An internally oxidized AgSnO 2 / In 2 O 3 material is also used. This material, described in DE-OS 24 28 147 , contains 5-10% SnO 2 and 1-6% In 2 O 3 .
  • a targeted change in the concentrations of the oxide additives to influence certain switching properties is often not always possible due to the oxidation kinetics.
  • a contact material which contains 1.6 to 6.5 Bi 2 O 3 and 0.1 to 7.5 SnO 2 in addition to silver.
  • This material can be produced both by internal oxidation and powder metallurgy.
  • Such high Bi 2 O 3 contents lead to embrittlement, so that the material can be produced only by individual sintering, but not by the more economical extrusion technology.
  • From the US 4,680,162 is an internally oxidized AgSnO 2 material is known, which may contain at tin contents of more than 4.5% additions of 0.1-5 indium and 0.01-5 bismuth.
  • the metal alloy powder is compacted and then internally oxidized. These additives inhibit the inhomogeneous oxide precipitations customary in internal oxidation. Optimal contact properties shows this Material not.
  • the powder metallurgical production of contact materials based on silver-tin oxide by mixing the powder, cold isostatic pressing, sintering and extrusion to semi-finished is, for example, from DE 43 19 137 and DE 43 31 526 known.
  • JP 50-19352 B1 shows a composite electrical contact material consisting of silver, cadmium oxide, magnesium oxide containing 0.1 to 0.3 wt .-% magnesium and tin oxide containing 2-4Gew .-% metallic tin, wherein a portion of magnesium and tin in the form of Mg 2 SnO 4 is present.
  • This object is achieved by a metal composite containing at least one metal and 5% to 60% by weight magnesium stannate, wherein the metal is silver or a silver alloy.
  • Magnesium stannate, Mg 2 SnO 4 is a compound known from the literature, the preparation of which is described, for example, in US Pat Materials in Electronics, 16 (2005), pages 193 to 196 .
  • the present patent application also relates to the use of a contact material containing at least one metal and magnesium stannate, wherein the metal is silver or a silver alloy, for the production of electrical contact pieces, as well as electrical contacts comprising such a contact material as further described.
  • the metal used is silver or silver alloys.
  • Silver alone also has excellent properties for many applications.
  • Cadmium on the other hand, is not included and may be present in the maximum range of unavoidable impurities.
  • at least 60% of the further oxide that is, for example, the tin oxide, particle sizes of 1 .mu.m or more, which is particularly advantageous in forming processes such as by extrusion.
  • the further oxide can also be used particle sizes of 20 nm to 2 microns or 50 nm to less than 2000 nm, in particular 100 nm to 1800 nm or 200 nm to 900 nm. In this case, advantageously 60% of the further oxide particle sizes of 100 nm to 900 nm.
  • the contact material can be obtained by a manufacturing method selected from powder metallurgy production, internal oxidation or combinations thereof.
  • magnesium stannate Mg 2 SnO 4 or a magnesium stannate precursor compound and optionally other oxides cold isostatic pressing the powder mixture, and sintering at temperatures of about 500 ° C to about 940 ° C and optionally forming the sintered material, such as by extrusion to wires or profiles, the contact material obtained.
  • Magnesiumstannat precursor compound of Magnesiumstannat various compounds can be used, which decompose under the process conditions in magnesium stannate and optionally further decomposition products.
  • the further decomposition products must either be volatile in the process conditions or be substances whose presence does not disturb the properties of the product obtained, ideally substances whose presence is desired, such as the metal used or another oxide selected from the group consisting of magnesium oxide, copper oxide, Bismuth oxide, tellurium oxide, tin oxide, indium oxide, tungsten oxide, molybdenum oxide or their combinations, their mixed oxides or combinations thereof.
  • Suitable compounds are, for example, alkoxides of tin and magnesium, such as hexakis [ ⁇ - (2-methyl-2-propanolato)] bis [(2-methyl-2-propanolato) tin] di-magnesium, CAS no. 139731-82-1.
  • the further oxide can also be used particle sizes of 20 nm to 2 microns or 50 nm to less than 2000 nm, in particular 100 nm to 1800 nm or 200 nm to 900 nm. In this case, advantageously 60% of the further oxide particle sizes of 100 nm to 900 nm.
  • the contact material can be obtained by a manufacturing method selected from powder metallurgy production, internal oxidation or combinations thereof.
  • magnesium stannate Mg 2 SnO 4 or a magnesium stannate precursor compound and optionally other oxides cold isostatic pressing the powder mixture, and sintering at temperatures of about 500 ° C to about 940 ° C and optionally forming the sintered material, such as by extrusion to wires or profiles, the contact material obtained.
  • Magnesiumstannat precursor compound of Magnesiumstannat various compounds can be used, which decompose under the process conditions in magnesium stannate and optionally further decomposition products.
  • the further decomposition products must either be volatile in the process conditions or be substances whose presence does not disturb the properties of the product obtained, ideally substances whose presence is desired, such as the metal used or another oxide selected from the group consisting of magnesium oxide, copper oxide, Bismuth oxide, tellurium oxide, tin oxide, indium oxide, tungsten oxide, molybdenum oxide or their combinations, their mixed oxides or combinations thereof.
  • Suitable compounds are, for example, alkoxides of tin and magnesium, such as, for example, hexakis [ ⁇ - (2-methyl-2-propanolato)] bis [(2-methyl-2-propanolato) tin] di-magnesium, CAS no. 139731-82-1.
  • too fine magnesium stannate or else other oxides can be coarsened by a heat treatment in which, for example, annealed at temperatures of about 700 ° C to about 1400 ° C until more than 60 wt.% Of magnesium stannate or other oxides have a particle size of more than 1 micron.
  • magnesium stannate (Mg 2 SnO 4 ) powders having smaller particle sizes may also be used, in which case additives such as sintering activators are advantageous, for example copper oxide CuO, nanoscale silver powder or other nanomaterials.
  • magnesium stannate can be used in which 60 wt.% Even before mixing with the metal powder have a particle size of at least 1 micron, but also magnesium stannate (Mg 2 SnO 4 ), in which 60% of magnesium stannate particle sizes of 50 nm to less than 1000 nm, in particular 60% of the magnesium stannate has particle sizes of 100 nm to 900 nm.
  • Mg 2 SnO 4 magnesium stannate
  • an alloy of silver with base metals is made pyrometallurgically and often heat-treated in pure oxygen under overpressure to form a contact material.
  • Such methods are known from the literature and described for example in EP 1505164 and EP 0508055 ,
  • a metal powder may be used which is e.g. contains further oxides which have been produced by internal oxidation, such as, for example, silver containing tin oxide.
  • the further processing then proceeds by powder metallurgy, that is to say by adding magnesium stannate and / or further oxides and / or metal powder, subsequent pressing, sintering and, if appropriate, shaping, such as, for example, Extrusion.
  • the contact material contains in particular silver and magnesium stannate and moreover only conventional impurities.
  • the contact material magnesium stannate in an amount of 0.2 to 20 wt .-% and ad 100 wt .-% silver and conventional impurities.
  • the contact material comprises magnesium stannate which has at least 60% of a particle size of 1 ⁇ m or more, in an amount of 0.2 to 20% by weight and ad 100% by weight of silver and conventional impurities.
  • the crushed powder mixture is calcined at 1400 ° C for 20 hours in air and then ground to a particle size (d50) of 2 microns (Fritsch Pulverisette 5, 2 mm ZrO 2 spheres, dry isopropanol).
  • d50 particle size of 2 microns
  • the resulting product was found to consist of 95.6% dimagnesium stannate (Mg 2 SnO 4 ) and 4.4% cassiterite (SnO 2 ).
  • FIG. 2 shows for both contact materials, which have an oxide content of 17.07 per cent by volume, the burnup in mg per switching operation.
  • the lower column shows the change at the fixed contact, the upper column at the moving contact. It can be seen that the magnesium stannate (Mg 2 SnO 4 ) and silver based contact material exhibits improved burn-off properties.
  • FIG. 3 shows the contact resistances in mOhms for both contact materials, which are given as mean values (in each case right column) and as 99% values. It can be seen that the averages are comparable but the 99% values are significantly lower for the magnesium stannate (Mg 2 SnO 4 ) and silver-based contact material and thus significantly improved over the silver-tin oxide material.
  • Mg 2 SnO 4 magnesium stannate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Contacts (AREA)
  • Powder Metallurgy (AREA)

Claims (14)

  1. Matériau de contact électrique sans cadmium, consistant en un métal et en 5 % en poids à 60 % en poids de stannate de magnésium Mg2SnO4, ainsi qu'en option et en outre en oxydes du groupe consistant en l'oxyde de magnésium, l'oxyde de cuivre, l'oxyde de bismuth, l'oxyde de tellure, l'oxyde d'étain, l'oxyde d'indium, l'oxyde de tungstène, l'oxyde de molybdène, les mélanges de ceux-ci ou les combinaisons de ceux-ci en des quantités de 0,5 % en poids à 30 % en poids, le métal étant l'argent ou un alliage d'argent.
  2. Matériau de contact selon la revendication 1, qui contient 0,2 à 60 pourcents en volume de stannate de magnésium.
  3. Matériau de contact selon l'une des revendications 1 à 2, dans lequel au moins 60 % en poids du stannate de magnésium présent dans le matériau de contact présente une granulométrie de 1 µm ou plus.
  4. Matériau de contact selon l'une ou plusieurs des revendications 1 à 3, dans lequel le stannate de magnésium présent dans le matériau de contact présente en totalité ou en partie une granulométrie de 20 nm à 1 µm.
  5. Matériau de contact selon l'une ou plusieurs des revendications 1 à 4, 60 % du stannate de magnésium présentant dans le matériau de contact une granulométrie de 100 nm à 900 nm.
  6. Matériau de contact selon l'une ou plusieurs des revendications 1 à 5, pouvant être obtenu par fabrication par métallurgie des poudres.
  7. Utilisation d'un matériau de contact selon l'une ou plusieurs des revendications 1 à 5 pour la fabrication de pièces de contact électriques.
  8. Contact électrique contenant un matériau de contact selon l'une ou plusieurs des revendications 1 à 5.
  9. Pièce de contact mobile d'un appareil de connexion ou appareil de connexion électrique, contenant un contact électrique selon la revendication 8.
  10. Procédé de fabrication d'un matériau de contact à partir d'un métal et de stannate de magnésium Mg2SnO4 selon l'une ou plusieurs des revendications 1 à 5 par mélange de stannate de magnésium pulvérulent Mg2SnO4 ou d'un composé précurseur de stannate de magnésium à la poudre métallique et éventuellement aux oxydes supplémentaires, pressage du mélange pour obtenir un comprimé, et frittage du comprimé pour obtenir un produit fritté.
  11. Procédé selon la revendication 10, dans lequel, dans une étape supplémentaire du procédé, on soumet la pièce frittée obtenue à un formage, en particulier à une extrusion.
  12. Procédé selon la revendication 10, dans lequel la pièce frittée est une pièce de contact.
  13. Procédé selon la revendication 10, dans lequel la pièce frittée contient en outre de l'oxyde de cuivre.
  14. Pièce de contact, pouvant être obtenue par un procédé selon la revendication 10 ou 11.
EP13715919.0A 2012-03-26 2013-03-26 Matière active composite Active EP2831298B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13715919.0A EP2831298B1 (fr) 2012-03-26 2013-03-26 Matière active composite

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP12161247.7A EP2644723B1 (fr) 2012-03-26 2012-03-26 Matière active composite
PCT/EP2013/056345 WO2013144112A1 (fr) 2012-03-26 2013-03-26 Matériau de contact
EP13715919.0A EP2831298B1 (fr) 2012-03-26 2013-03-26 Matière active composite

Publications (2)

Publication Number Publication Date
EP2831298A1 EP2831298A1 (fr) 2015-02-04
EP2831298B1 true EP2831298B1 (fr) 2019-05-08

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Application Number Title Priority Date Filing Date
EP12161247.7A Not-in-force EP2644723B1 (fr) 2012-03-26 2012-03-26 Matière active composite
EP13715919.0A Active EP2831298B1 (fr) 2012-03-26 2013-03-26 Matière active composite

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EP12161247.7A Not-in-force EP2644723B1 (fr) 2012-03-26 2012-03-26 Matière active composite

Country Status (4)

Country Link
US (1) US9928931B2 (fr)
EP (2) EP2644723B1 (fr)
CN (1) CN104245976B (fr)
WO (1) WO2013144112A1 (fr)

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CN103613118B (zh) * 2013-11-15 2015-08-19 广东光华科技股份有限公司 一种高纯度锡酸镁粉体的制备方法
CN103681015B (zh) * 2013-11-28 2015-12-02 昆明理工大学 一种复相金属氧化物增强银基电触头材料的制备方法
CN103710556B (zh) * 2013-12-27 2015-08-05 桂林电器科学研究院有限公司 一种粉末轧制法制备银氧化锡触头材料的工艺
US10699851B2 (en) * 2016-06-22 2020-06-30 Teledyne Scientific & Imaging, Llc Sintered electrical contact materials
US10290434B2 (en) 2016-09-23 2019-05-14 Honeywell International Inc. Silver metal oxide alloy and method of making
CN115537594B (zh) * 2022-10-28 2023-04-25 台州慧模科技有限公司 一种银基电触头材料及其制备方法

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Publication number Publication date
CN104245976A (zh) 2014-12-24
CN104245976B (zh) 2017-06-09
EP2831298A1 (fr) 2015-02-04
EP2644723A1 (fr) 2013-10-02
WO2013144112A1 (fr) 2013-10-03
US9928931B2 (en) 2018-03-27
EP2644723B1 (fr) 2017-01-18
US20150060741A1 (en) 2015-03-05

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