EP1584696A1 - HERSTELLUNGSVERFAHREN FÜR ELEKTRISCHES KONTAKTMATERIAL AUF Ag-OXIDBASIS UND DESSEN PRODUKT - Google Patents

HERSTELLUNGSVERFAHREN FÜR ELEKTRISCHES KONTAKTMATERIAL AUF Ag-OXIDBASIS UND DESSEN PRODUKT Download PDF

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Publication number
EP1584696A1
EP1584696A1 EP02762779A EP02762779A EP1584696A1 EP 1584696 A1 EP1584696 A1 EP 1584696A1 EP 02762779 A EP02762779 A EP 02762779A EP 02762779 A EP02762779 A EP 02762779A EP 1584696 A1 EP1584696 A1 EP 1584696A1
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EP
European Patent Office
Prior art keywords
weight
oxide
internal
electric contact
temperature
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.)
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Application number
EP02762779A
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English (en)
French (fr)
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EP1584696A4 (de
EP1584696B1 (de
Inventor
Sadao c/o Tokuriki Honten Co. Ltd. SATO
Hideo c/o Tokuriki Honten Co. Ltd. KUMITA
Kohei c/o Tokuriki Honten Co. Ltd. TSUDA
Mitsuo c/o Fuji Electric Co. Ltd. YAMASHITA
Kunio c/o Fuji Electric Co. Ltd. SHIOKAWA
Kenichi c/o Fuji Electric Co. Ltd. KAMIURA
Kiyoshi c/o Fuji Electric Co. Ltd. SEKIGUCHI
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tokuriki Honten Co Ltd
Fuji Electric FA Components and Systems Co Ltd
Original Assignee
Tokuriki Honten Co Ltd
Fuji Electric FA Components and Systems Co Ltd
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Publication date
Application filed by Tokuriki Honten Co Ltd, Fuji Electric FA Components and Systems Co Ltd filed Critical Tokuriki Honten Co Ltd
Priority to AT02762779T priority Critical patent/ATE344841T1/de
Publication of EP1584696A4 publication Critical patent/EP1584696A4/de
Publication of EP1584696A1 publication Critical patent/EP1584696A1/de
Application granted granted Critical
Publication of EP1584696B1 publication Critical patent/EP1584696B1/de
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    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • 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

Definitions

  • This invention relates to an Ag-oxide-based electric contact material having excellent contact reliability, deposition resistance and arc resistance, used for various switches, contactors, breakers and the like, and a method for manufacturing the same.
  • Ag-CdO-based materials have excellent electric properties such as deposition resistance, arc resistance and low contact resistance and therefore there has been a large demand for Ag-CdO-based materials in various fields. These materials have been improved over a long time and many academic researches on these materials have been conducted. These materials and manufacturing techniques have reached, so to speak, the maximum.
  • anAg-(Sn, In, Sb) -based internal oxidation contact material has been developed as a medium-load contact having various properties.
  • recent devices are miniaturized very rapidly and more strict properties, particularly of a contact, are demanded.
  • an internal structure having an oxide precipitated and dispersed therein is provided.
  • an Ag-rich layer formed on the surface at the time of preparing a contact and an oxide-flocculated layer that is immediately below the Ag-rich layer cause adverse effects such as deposition and increase in temperature of the contact at the time of opening/closing of the contact.
  • the inventor analyzed various elements causing the temperature, oxygen pressure and added element in the internal oxidation mechanism to change the oxidized structure and also reviewed the manufacturing conditions with a broader scope of analysis. Moreover, the inventor reconsidered the contribution of various elements other than Cd to the contact property of the oxide and analyzed various phenomena with respect to a cleaning effect and arc on the surface of an electric contact, for example, properties of an oxide to be added, particularly the temperature characteristic of its steam pressure and the relation between the state of dispersion in Ag and an arc-suppressing phenomenon in an arc generated at the time of opening/closing. Thus, the inventor could confirm the optimum relation of the dispersion in Ag of an oxide containing an added element and composite oxide having electric properties such as deposition resistance, arc resistance and low contact resistance that are equivalent to those of an Ag-CdO-based electric contact material.
  • the inventor also confirmed that dispersion of composite oxides of added elements other than Sn into Ag provides a synergistic effect.
  • the present invention is provided on the basis of the above-described confirmation.
  • the present invention is characterized in that an oxide of In having a low steam pressure than CdO within a temperature range of approximately 500 to 4000°C is dispersed in an Sn oxide, thereby making the behavior of a synthetic steam pressure of these oxides in the form of a metal composite oxide more approximate to the behavior of the steam pressure of CdO so that their synergistic effect provides excellent contact properties.
  • the present invention is also characterized in that as a measure for restraining generation of an Ag-rich layer on the outermost surface of the contact, which is considered to make the contact reliability of the contact unstable, an alloy made of Sn at a rate of 1 to 5% by weight, In at 3 to 10% by weight, one or two types of Fe, Ni and Co at 0.05 to 1% by weight and Ag for the remaining part is internally oxidized in Ag, and the Sn-In composite oxide of the added elements and oxides of one or two types of Fe, Ni and Co are uniformly and finely precipitated and dispersed in the internal structure.
  • the present invention is characterized in that an oxide of In having a low steam pressure than CdO within a temperature range of approximately 500 to 4000°C is dispersed in Sn and Bi oxides, thereby making the behavior of a synthetic steam pressure of these oxides in the form of a metal composite oxide more approximate to the behavior of the steam pressure of CdO so that their synergistic effect provides excellent contact properties.
  • the present invention is also characterized in that as a measure for restraining generation of an Ag-rich layer on the outermost surface of the contact, which is considered to make the contact reliability of the contact unstable, an alloy made of Sn at a rate of 1 to 5% by weight, In at 3 to 10% by weight, Bi at 0.05 to 2% by weight, one or two types of Fe, Ni and Co at 0.05 to 1% by weight and Ag for the remaining part is internally oxidized, and the Sn-In composite oxide, In-Bi composite oxide, Sn-Bi composite oxide and Sn-In-Bi composite oxide of the added elements and oxides of one or two types of Fe, Ni and Co are uniformly and finely precipitated and dispersed in the internal structure.
  • the present invention is characterized in that an oxide of In having a low steam pressure than CdO within a temperature range of approximately 500 to 4000°C is dispersed in Sn and Sb oxides, thereby making the behavior of a synthetic steam pressure of these oxides in the form of a metal composite oxide more approximate to the behavior of the steam pressure of CdO so that their synergistic effect provides excellent contact properties.
  • the present invention is also characterized in that as a measure for restraining generation of an Ag-rich layer on the outermost surface of the contact, which is considered to make the contact reliability of the contact unstable, an alloy made of Sn at a rate of 1 to 5% by weight, In at 3 to 10% by weight, Sb at 0.05 to 5% by weight, one or two types of Fe, Ni and Co at 0.05 to 1% by weight and Ag for the remaining part is internally oxidized, and the Sn-In composite oxide, In-Sb composite oxide, Sn-Sb composite oxide and Sn-In-Sb composite oxide of the added elements and oxides of one or two types of Fe, Ni and Co are uniformly and finely precipitated and dispersed in the internal structure.
  • the present invention is characterized in that an oxide of In having a lower steam pressure than CdO within a temperature range of approximately 500 to 4000°C is dispersed in Sn, Bi and Sb oxides, thereby making the behavior of a synthetic steam pressure of these oxides in the form of a metal composite oxide more approximate to the behavior of the steam pressure of CdO so that their synergistic effect provides excellent contact properties.
  • the present invention is also characterized in that as a measure for restraining generation of an Ag-rich layer on the outermost surface of the contact, which is considered to make the contact reliability of the contact unstable, an alloy made of Sn at a rate of 1 to 5% by weight, In at 3 to 10% by weight, Bi at 0.05 to 2% by weight, Sb at 0.05 to 5% by weight, one or two types of Fe, Ni and Co at 0.05 to 1% by weight and Ag for the remaining part is internally oxidized, and the Sn-In composite oxide, In-Bi composite oxide, Sn-Bi composite oxide, Sn-Sb composite oxide, In-Sb composite oxide and Sn-In-Bi-Sb composite oxide of the added elements and oxides of one or two types of Fe, Ni and Co are uniformly and finely precipitated and dispersed in the internal structure.
  • an alloy made by solving Sn, In and one or two types of Fe, Ni and Co, and if necessary, one type or more of Bi and Sb, into Ag is prepared in a desired contact shape at a processing rate of 50 to 95%, and after replacement with pure oxygen under a normal pressure, the temperature is raised from 200°C in an oxygen atmosphere with an oxygen pressure of 5 to 50 kg/cm 2 to set an internal oxidation temperature with an upper limit of 700°C.
  • generation of an Ag-rich layer and an oxide-flocculated layer immediately below the Ag-rich layer, which are generated in the progress of internal oxidation of the conventional process is restrained, and the internal dislocation density is increased by intense processing at the above-described high processing rate.
  • the composite oxides of the added elements are uniformly and finely precipitated and dispersed into the deep internal structure. This can provide a Cd-free electric contact having excellent electric properties such as deposition resistance, arc resistance and low contact resistance.
  • the reason for setting the upper limit of the processing rate at 95% is that further processing is difficult in consideration of the limit of the processability of the material while processing at less than 50% is insufficient for generation of a sufficiently effective processing strain.
  • the reason for the replacement with pure oxygen under a normal temperature and setting the oxygen pressure at 5 to 50 kg/cm 2 is that the replacement removes non-oxidative gases in the internal oxidation furnace, that is, nitrogen and hydrogen in the air, to improve the oxidation atmosphere in the furnace and that an oxygen pressure less than 5 kg/cm 2 is insufficient to realize uniform and fine precipitation and dispersion of the composite oxides of the added elements to the deep part in the material while an oxygen pressure equal to or higher than 50 kg/cm 2 increases the scale of the furnace facility and cannot provide an outstanding effect on the properties that matches the manufacturing cost.
  • the reason for raising the temperature from 200° in the pressured oxygen atmosphere and setting the internal oxidation temperature with the upper limit of 700°C is that 200°C is the lower limit of the temperature range of internal oxidation while at a temperature equal to or higher than 700°C, the diffusion rate of the solute element becomes higher than the diffusion rate of oxygen from the material surface in internal oxidation, thus forming solid layered flocculation on the surface layer of the structure and obstructing the subsequent progress of internal oxidation.
  • the reason for setting the upper limit of the content range of Sn with respect to Ag at 5% by weight is that addition exceeding this limit cannot realize fine precipitation of the oxide and forms solid layered flocculation inside the oxidized structure, thus obstructing the subsequent progress of internal oxidation and causing serious fragility in the oxidized structure.
  • addition less than 1% by weight cannot satisfy composite oxidation with many elements and cannot provide an addition effect for sufficient electric properties.
  • the reason for setting the upper limit of the content range of In at 10% by weight is that addition exceeding this limit forms a fine oxide coating on the surface in combination with the other elements at the time of internal oxidation and makes entry of oxygen from the surface difficult.
  • Addition less than 3% by weight cannot realize the restraining effect on volatile damage and exhaustion due to an arc, that is, the effect of the above-described lower steam pressure than that of CdO.
  • the reason for setting the upper limit of the content range of Bi at 2% by weight is that addition exceeding this limit causes hot fragility and makes it difficult to prepare an alloy for making a finer oxide, which is an element of the present invention, at a processing rate of 50 to 95%.
  • addition causes significant flocculation of the oxide at the time of internal oxidation and obstructs the subsequent progress of internal oxidation.
  • Addition less than 0.05% by weight does not realize the effect to finely disperse the composite oxide particles.
  • the reason for setting the upper limit of the content range of Sb at 5% by weight is that addition exceeding this limit forms a fine oxide coating on the surface in combination with the other elements at the time of internal oxidation and makes entry of oxygen from the surface difficult. Addition less than 0.05% by weight does not realize the contact surface cleaning effect, which is the effect of the higher steam pressure than that of CdO.
  • the addition of one or two types of Fe, Ni and Co is effective mainly for making finer crystal grains and equalizing the oxide particle size.
  • the reason for setting the upper limit of this addition at 1% by weight is that alloying by a melting method is extremely difficult even when addition exceeding this limit is performed, whereas addition less than 0.05% by weight cannot realize the effect to make finer crystal grains and the like.
  • composition alloys shown in Fig.3 were prepared by the following process.
  • the temperature of this sample was raised to 200 to 600°C in an oxidation atmosphere with an oxygen pressure of 50 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 630°C in an oxidation atmosphere with an oxygen pressure of 30 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 550°C in an oxidation atmosphere with an oxygen pressure of 5 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 700°C in an oxidation atmosphere with an oxygen pressure of 50 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 670°C in an oxidation atmosphere with an oxygen pressure of 5 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 650°C in an oxidation atmosphere with an oxygen pressure of 20 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 600°C in an oxidation atmosphere with an oxygen pressure of 10 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 680°C in an oxidation atmosphere with an oxygen pressure of 8 kg/cm 2 , thus internally oxidizing the sample.
  • the temperature was raised to 200 to 450°C in an oxidation atmosphere with an oxygen pressure of 40 kg/cm 2 , thus internally oxidizing the sample.
  • an alloy containing Ag and 12% by weight of Cd as conventional example 1 an alloy containing Ag, 6% by weight of Sn and 3% by weight of In as conventional example 2, and an alloy containing Ag and 7% by weight of In as conventional example 3 were prepared and formed in a similar shape at a processing rate of 50% or less, and then internally oxidized at a fixed temperature of 780°C in an oxidation atmosphere with an oxygen pressure of 3 kg/cm 2 .
  • an actual machine test (AC 200V and 20A) was carried out using a contact resistor, a deposition tester (rated at 60A) and a commercially available contactor, and the electric properties were evaluated.
  • the present invention is effective for removing the Ag-rich layer appearing on the outermost surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Contacts (AREA)
  • Manufacture Of Switches (AREA)
EP02762779A 2002-08-15 2002-08-15 HERSTELLUNGSVERFAHREN FÜR ELEKTRISCHES KONTAKTMATERIAL AUF Ag-OXIDBASIS UND DESSEN PRODUKT Expired - Lifetime EP1584696B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT02762779T ATE344841T1 (de) 2002-08-15 2002-08-15 Herstellungsverfahren für elektrisches kontaktmaterial auf ag-oxidbasis und dessen produkt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2002/008294 WO2004016818A1 (ja) 2001-06-01 2002-08-15 Ａｇ−酸化物系電気接点材料の製造方法およびその製品

Publications (3)

Publication Number Publication Date
EP1584696A4 EP1584696A4 (de) 2005-10-12
EP1584696A1 true EP1584696A1 (de) 2005-10-12
EP1584696B1 EP1584696B1 (de) 2006-11-08

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EP02762779A Expired - Lifetime EP1584696B1 (de) 2002-08-15 2002-08-15 HERSTELLUNGSVERFAHREN FÜR ELEKTRISCHES KONTAKTMATERIAL AUF Ag-OXIDBASIS UND DESSEN PRODUKT

Country Status (3)

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EP (1) EP1584696B1 (de)
DE (1) DE60215981T2 (de)
WO (1) WO2004016818A1 (de)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3874941A (en) * 1973-03-22 1975-04-01 Chugai Electric Ind Co Ltd Silver-metal oxide contact materials
EP0508055A1 (de) * 1991-04-12 1992-10-14 Mitsubishi Materials Corporation Auf Silberoxid basierendes elektrisches Kontaktmaterial
EP0877403A1 (de) * 1995-10-12 1998-11-11 Omron Corporation Schalter

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS542234A (en) * 1977-06-08 1979-01-09 Tanaka Precious Metal Ind Method of making electric contact material consisting of silverrtinoxide base alloy
JPS58100650A (ja) * 1981-12-11 1983-06-15 Matsushita Electric Ind Co Ltd 電気接点材料
JPS59219432A (ja) * 1983-05-27 1984-12-10 Chugai Electric Ind Co Ltd 銀−錫酸化物系複合接点材とその製法
JPS62241207A (ja) * 1986-04-11 1987-10-21 中外電気工業株式会社 電気接点材料
JPH0989727A (ja) * 1995-09-21 1997-04-04 Matsushita Electric Works Ltd 大気成分捕集器

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3874941A (en) * 1973-03-22 1975-04-01 Chugai Electric Ind Co Ltd Silver-metal oxide contact materials
EP0508055A1 (de) * 1991-04-12 1992-10-14 Mitsubishi Materials Corporation Auf Silberoxid basierendes elektrisches Kontaktmaterial
EP0877403A1 (de) * 1995-10-12 1998-11-11 Omron Corporation Schalter

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO2004016818A1 *

Also Published As

Publication number Publication date
DE60215981T2 (de) 2007-07-26
DE60215981D1 (de) 2006-12-21
EP1584696A4 (de) 2005-10-12
EP1584696B1 (de) 2006-11-08
WO2004016818A1 (ja) 2004-02-26

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